AN ABSTRACT OF THE THESIS OF Melissa M. Sales for the degree of Master of Science in Food Science and Technology presented on July 25, 2013 Title: An Evaluation of Blackberry Harvest Sanitation and the Ability of Foodborne Pathogens to Survive in Blackberry Products Abstract approved: Mark A. Daeschel Blackberries, genus Rubus, are an important Oregon agricultural commodity. In their fresh and processed forms, they offer many health benefits and may be able to help Americans better achieve fruit consumption recommendations because of convenience and pleasant sensory qualities. However, the susceptibility of blackberry products to contamination with bacterial pathogens of human health concern is unknown. Blackberries have never directly been implicated in a food safety incident; however, raspberries, also in the Rubus genus, have been the vehicle for hepatitis A, norovirus, and Cyclospora cayetanensis outbreaks. Furthermore, strawberries were recently the source of an Escherichia coli O157:H7 outbreak in Oregon. To better understand the potential for microbial pathogen contamination and the ability of these microorganisms to survive or grow in blackberry products, several studies were conducted. Fresh berries from the ‘Obsidian’ and ‘Triple Crown’ cultivars were evaluated at different harvest periods for the aerobic plate count, coliforms, yeasts, and molds to establish a baseline microbial population. Environmental samples were taken from a clean mechanical harvester and then from the same harvester that had been intentionally left soiled with berry harvest debris to determine the impact of harvester microbial quality. Samples from ‘Marion’ and ‘Black Diamond’ cultivars were hand harvested and evaluated for E. coli O157:H7 and Salmonella spp. by rapid detection methods via the NEOGEN® Reveal® 2.0 systems. Fresh, wild ‘Himalaya’ blackberries and frozen blackberries from the ‘Triple Crown’ cultivar were spot inoculated with Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus to determine the ability of these microorganisms to survive on the berry surface. ‘Himalaya’ samples were stored for 3 days at ambient temperatures and ‘Triple Crown’ for 6 months at -23.3°C. Lastly, juice and wine were made from ‘Marion’ and ‘Black Diamond’ purees. The juices and wines were used for pathogen survival studies using the aforementioned microorganisms to better understand what constituents of blackberries may contribute to bactericidal effects, as well as the survival patterns in these products. Aerobic plate counts for ‘Obsidian’ and ‘Triple Crown’ cultivars ranged from 3.524.62 log CFU/g of berry with later harvests tending to have higher values. ‘Triple Crown’ mid-late harvest samples were significantly higher than the early harvest samples (p = 0.005). Yeasts and molds ranged from 3.01-4.73 log CFU/g of berry with later harvests having significantly higher values for both cultivars (p = 0.048 ‘Obsidian’; p <0.001 ‘Triple Crown’). Coliforms were detected in ‘Obsidian’ mid-harvest and ‘Triple Crown’ earlyharvest samples at 2.10 and 1.40 log CFU/g of berry, respectively. The aerobic plate counts measured from the clean and intentionally soiled mechanical harvester were not significantly different. Escherichia coli O157:H7 and Salmonella spp. were not detected using rapid detection methods in evaluated ‘Marion’ and ‘Black Diamond’ samples. Escherichia coli O157:H7 was not detectable in fresh or frozen inoculated samples. Salmonella Typhimurium was detected in 2 frozen samples with 2.95 and 3.21 log reductions. Listeria monocytogenes was only detected in frozen samples and experienced log reductions ≥ 2.42. Staphylococcus aureus was detectable on every fresh and frozen berry inoculated with log reductions ranging from 0.67 to 3.48. The greatest reductions occurred with fresh samples. Growth of microorganisms was not observed in any juice or wine samples. Maximum observed survival times in juices ranged from 12 h for L. monocytogenes to 108 h for Salmonella Typhimurium. Maximum survival times in wines were 40 m for both E. coli O157:H7 and Salmonella Typhimurium, and 80 m for both L. monocytogenes and S. aureus. Adding ethanol to juice samples to equal that of their counterpart wines decreased survival time for all microorganisms evaluated by several hours. Increasing the pH of wines by approximately one unit increased the survival time from minutes to hours, and in some cases, days. The overall results suggest that blackberries are not an ideal environment for E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus to grow. However, these microorganisms may be able to survive depending on the type of blackberry product and its subsequent storage. Many constituents of blackberries may provide bactericidal activity, with organic acids appearing to have the greatest effect. ©Copyright by Melissa M. Sales July 25, 2013 All Rights Reserved An Evaluation of Blackberry Harvest Sanitation and the Ability of Foodborne Pathogens to Survive in Blackberry Products by Melissa M. Sales A THESIS Submitted to Oregon State University in partial fulfillment of the requirements for the degree of Master of Science Presented July 25, 2013 Commencement June 2014 Master of Science thesis of Melissa M. Sales presented on July 25, 2013. APPROVED: Major Professor, representing Food Science and Technology Head of the Department of Food Science and Technology Dean of the Graduate School I understand that my thesis will become part of the permanent collection of Oregon State University libraries. My signature authorizes release of thesis to any reader upon request. Melissa M. Sales, Author ACKNOWLEDGEMENTS I would like to express my sincerest gratitude to Mark Daeschel, not only for being an incredibly patient and compassionate mentor, but for also giving me the freedom and opportunities to discover my strengths. For that, I am truly grateful. Thank you to David Bryla, Javier Fernandez-Salvador, Renee Harkins, Angela Tseng, Jooyeoun Jung, George Cavender and Mingyang Lui for all of their time, knowledge, and assistance with collecting samples. I would like to thank everyone that gave me support and advice during my time at OSU, especially Dan Smith, Linda Dunn, Lisbeth Goddik, Joy Waite-Cusic, Brian Yorgey, and Jeff Clawson. Whether you know it or not, you’ve made many decisions that I’ve had to make a little easier. Thank you to all of the wonderful and supportive friends that I have made at OSU that I have come to consider family. I would especially like to thank Jake Mattson for teaching me not to take myself too seriously and for helping me to become a larger geek than I ever could have become on my own. I would like to thank my significant other, Zak, for his incredible support and for never giving up on me during my academic journey even when I was completely insufferable. I would also like to thank my son, Alex, for being the greatest, most patient kid I could have ever asked for and for giving me a reason to establish higher goals. I only wish that my parents, Karen and Gilbert Sales, could have seen me come this far. CONTRIBUTION OF AUTHORS Dr. Joy Waite-Cusic assisted with microbiological data interpretation. Jacob Mattson assisted with the statistical analysis of harvester and microflora data. TABLE OF CONTENTS Page 1. Introduction .................................................................................................................... 1 1.1 Production ................................................................................................................. 1 1.2 Consumption and Health Benefits ............................................................................ 2 1.3 Potential microbial Risks ........................................................................................... 6 1.4 Potential Antimicrobial Properties .......................................................................... 10 2. An Evaluation of Blackberry Harvest Sanitation and the Ability of Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus to Survive on the Surface of Fresh and Frozen Blackberry Fruit ...................................... 13 2.1 Abstract ................................................................................................................... 14 2.2 Introduction............................................................................................................. 16 2.3 Materials and Methods ........................................................................................... 20 2.3.1 Fresh Field Samples .......................................................................................... 20 2.3.2 Direct Pathogen Testing ................................................................................... 21 2.3.3 Mechanical Harvester ....................................................................................... 22 2.3.4 Whole Berry Inoculation................................................................................... 23 2.3.5 Data Analysis..................................................................................................... 25 2.4 Results and Discussion ............................................................................................ 25 2.4.1 Fresh Field Data ................................................................................................ 25 2.4.2 Direct Pathogen Testing ................................................................................... 28 2.4.3 Mechanical Harvester ....................................................................................... 29 2.4.4 Spot Inoculation Studies ................................................................................... 30 2.5 Conclusions.............................................................................................................. 35 3. An Evaluation of the Survival of Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus in ‘Marion’ and ‘Black Diamond’ Blackberry Juice and Wine ................................................................................................ 37 TABLE OF CONTENTS (Continued) 3.1 Abstract ................................................................................................................... 38 3.2 Introduction............................................................................................................. 39 3.3 Materials and Methods ........................................................................................... 42 3.3.1 Juice and Wine Preparation.............................................................................. 42 3.3.2 Juice and Wine Properties ................................................................................ 43 3.3.3 Culture Preparation .......................................................................................... 43 3.3.4 Survival Study Procedure .................................................................................. 44 3.3.5 Data Analysis..................................................................................................... 44 3.4 Results and Discussion ............................................................................................ 44 3.4.1 Properties of Purees, Juices, and Wines........................................................... 44 3.4.2 Survival Study Results ....................................................................................... 45 3.5 Conclusions.............................................................................................................. 55 4. Overall Conclusions and Future Work ......................................................................... 57 Bibliography ...................................................................................................................... 59 APPENDICES ...................................................................................................................... 65 LIST OF FIGURES Figure Page Figure 2.1 Aerobic Plate Count at Various Harvest Times ................................................ 27 Figure 2.2 Yeasts and Molds at Various Harvest Times .................................................... 27 Figure 2.3 Coliforms at Various Harvest Times ................................................................. 28 Figure 2.4 Mechanical Harvester Aerobic Plate Counts ................................................... 29 Figure 3.1 Survival of E. coli O157:H7 in ‘Marion’ Products ............................................. 48 Figure 3.2 Survival of E. coli O157:H7 in ‘Marion’ Wine ................................................... 49 Figure 3.3 Survival of E. coli O157:H7 in ‘Black Diamond’ Products ................................ 49 Figure 3.4 Survival of E. coli O157:H7 in ‘Black Diamond’ Wine ...................................... 50 Figure 3.5 Survival of Salmonella Typhimurium in ‘Marion’ Products ............................ 50 Figure 3.6 Survival of Salmonella Typhimurium in ‘Marion’ Wine ................................... 51 Figure 3.7 Survival of Salmonella Typhimurium in ‘Black Diamond’ Products ................. 51 Figure 3.8 Survival of Salmonella Typhimurium in ‘Black Diamond’ Wine....................... 52 Figure 3.9 Survival of S. aureus in ‘Marion’ Products ....................................................... 53 Figure 3.10 Survival of S. aureus in ‘Marion’ Wine ........................................................... 53 Figure 3.11 Survival of S. aureus in ‘Black Diamond’ Products......................................... 54 Figure 3.12 Survival of S. aureus in ‘Black Diamond’ Wine .............................................. 54 LIST OF TABLES Table Page Table 2.1 Cultivar Information .......................................................................................... 17 Table 2.2 Detection of E. coli O157:H7 and Salmonella spp. in ‘Marion’ and ‘Black Diamond’ Cultivars ............................................................................................................ 28 Table 2.3 ‘Himalaya’ inoculated with E. coli O157:H7 ...................................................... 30 Table 2.4 ‘Himalaya’ inoculated with Salmonella Typhimurium ...................................... 31 Table 2.5 ‘Himalaya’ inoculated with L. monocytogenes ................................................. 31 Table 2.6 ‘Himalaya’ inoculated with S. aureus ............................................................... 31 Table 2.7 Frozen ‘Triple Crown’ inoculated with E. coli O157:H7 .................................... 32 Table 2.8 Frozen ‘Triple Crown’ inoculated with Salmonella Typhimurium ................... 33 Table 2.9 Frozen ‘Triple Crown’ inoculated with L. monocytogenes ................................ 33 Table 2.10 Frozen ‘Triple Crown’ inoculated with S. aureus ............................................ 34 Table 3.1 Cultivar Information ......................................................................................... 39 Table 3.2 pH and Soluble Solid Content of Blackberry Puree .......................................... 45 Table 3.3 pH, Soluble Solid Content, and Titratable Acidity of Blackberry Juices ............ 45 Table 3.4 pH, Ethanol Content, and Titratable Acidity of Blackberry Wines .................... 45 Table 3.5 Maximum Observed Survival Times of L. monocytogenes in ‘Marion’ and ‘Black Diamond’ Juices and Wines: All Treatments .................................................................... 52 LIST OF APPENDICES Appendix Page Appendix I. Fresh Field Samples Raw Data, Chapter 2 .................................................... 66 Appendix II. Mechanical Harvester Raw Data and Photos, Chapter 2 ............................ 69 Appendix III. ‘Himalaya’ Raw Data, Chapter 2 ...................................................................... 72 Appendix IV. ‘Triple Crown’ Raw Data, Chapter 2 ................................................................ 74 Appendix V. Juice Raw Data, Chapter 3 ................................................................................ 80 Appendix VI. Juice Variables Raw Data, Chapter 3 ................................................................ 89 Appendix VII. Wine Raw Data, Chapter 3 ............................................................................... 94 Appendix VIII. Wine Variable Raw Data, Chapter 3 .............................................................. 102 Appendix IX. Inocula Raw Data, Chapter 3 .......................................................................... 107 LIST OF APPENDIX FIGURES Figure Page Figure II.1 Harvester Location 1 ........................................................................................ 70 Figure II.2 Harvester Location 2 ...................................................................................... 70 Figure II-3 Harvester Location 3 ...................................................................................... 71 Figure II.4 Harvester Location 4 ...................................................................................... 71 Figure II.5 Harvester Location 5 ........................................................................................ 71 Figure II.6 Harvester Location 6 ........................................................................................ 71 Figure II.7 Harvester Location 7 ........................................................................................ 72 Figure II.8 Harvester Location 8 ........................................................................................ 72 LIST OF APPENDIX TABLES Table Page Table I.1 Aerobic Plate Count Raw Data, Fresh Samples .................................................. 66 Table I.2 Yeasts and Molds Raw Data, Fresh Samples ...................................................... 67 Table I.3 Coliforms Raw Data, Fresh Samples ................................................................... 68 Table II.1 Aerobic Plate Count Raw Data .......................................................................... 69 Table III.1 E. coli O157:H7 on fresh 'Himalaya' Blackberries, Raw Data ....................... 72 Table III.2 Salmonella Typhimurium on fresh 'Himalaya' Blackberries, Raw Data ......... 73 Table III.3 L. monocytogenes on fresh 'Himalaya' Blackberries, Raw Data ...................... 73 Table III.4 S. aureus on fresh 'Himalaya' Blackberries, Raw Data ..................................... 74 Table IV.1 E. coli O157:H7 on Frozen 'Triple Crown' Blackberries, Raw Data ................ 74 Table IV.2 Salmonella Typhimurium on Frozen 'Triple Crown' Blackberries, Raw Data . 76 Table IV.3 L. monocytogenes on Frozen 'Triple Crown' Blackberries, Raw Data ............ 77 Table IV.4 S. aureus on Frozen 'Triple Crown' Blackberries, Raw Data ............................ 78 Table V.1 E. coli O157:H7 in 'Marion' Juice, Raw Data ..................................................... 80 Table V.2 E. coli O157:H7 in 'Black Diamond' Juice, Raw Data ......................................... 81 Table V.3 Salmonella Typhimurium in 'Marion' Juice, Raw Data ..................................... 82 Table V.4 Salmonella Typhimurium in 'Black Diamond' Juice, Raw Data ......................... 83 Table V.5 L. monocytogenes in 'Marion' Juice, Raw Data................................................. 85 Table V.6 L. monocytogenes in 'Black Diamond' Juice, Raw Data .................................... 86 Table V.7 S. aureus in 'Marion' Juice, Raw Data ............................................................... 87 LIST OF APPENDIX TABLES (Continued) Table Page Table V.8 S. aureus in 'Black Diamond' Juice, Raw Data ................................................... 87 Table VI.1 E. coli O157:H7 in 'Marion' Juice with added ethanol, Raw Data.................... 89 Table VI.2 E. coli O157:H7 in 'Black Diamond' Juice with added ethanol, Raw Data ....... 90 Table VI.3 Salmonella Typhimurium in 'Marion' Juice with added ethanol, Raw Data .... 90 Table VI.4 Salmonella Typhimurium in 'Black Diamond' Juice with added ethanol, Raw Data ................................................................................................................................... 91 Table VI.5 L. monocytogenes in 'Marion' Juice with added ethanol, Raw Data ............... 91 Table VI.6 L. monocytogenes in 'Black Diamond' Juice with added ethanol, Raw Data... 92 Table VI.7 S. aureus in 'Marion' Juice with added ethanol, Raw Data ............................. 92 Table VI.8 S. aureus in 'Black Diamond' Juice with added ethanol, Raw Data ............... 93 Table VII.1 E. coli O157:H7 in 'Marion' Wine, Raw Data ................................................. 94 Table VII.2 E. coli O157:H7 in 'Black Diamond' Wine, Raw Data ...................................... 95 Table VII.3 Salmonella Typhimurium in 'Marion' Wine, Raw Data ................................... 96 Table VII. 4 Salmonella Typhimurium in 'Black Diamond' Wine, Raw Data ..................... 96 Table VII.5 L. monocytogenes in 'Marion' Wine, Raw Data ............................................ 97 Table VII.6 L. monocytogenes in 'Black Diamond' Wine, Raw Data ................................ 98 Table VII.7 S. aureus in 'Marion' Wine, Raw Data ............................................................ 99 Table VII.8 S. aureus in 'Black Diamond' Wine, Raw Data ............................................ 100 Table VIII.1 E. coli O157:H7 in pH adjusted 'Marion' Wine, Raw Data ......................... 102 Table VIII.2 E. coli O157:H7 in pH adjusted 'Black Diamond' Wine, Raw Data ............. 103 LIST OF APPENDIX TABLES (Continued) Table Page Table VIII.3 Salmonella Typhimurium in pH adjusted 'Marion' Wine, Raw Data ........... 103 Table VIII.4 Salmonella Typhimurium in pH adjusted 'Black Diamond' Wine, Raw Data 104 Table VIII.5 L. monocytogenes in pH adjusted 'Marion' Wine, Raw Data ..................... 104 Table VIII.6 L. monocytogenes in pH adjusted 'Black Diamond' Wine, Raw Data ........ 105 Table VIII.7 S. aureus in pH adjusted 'Marion' Wine, Raw Data ................................... 106 Table VIII.8 S. aureus in pH adjusted 'Black Diamond' Wine, Raw Data ....................... 106 Table IX.1 Inocula for Juice Survival Studies ................................................................... 107 Table IX.2 Inocula for Wine Survival Studies .................................................................. 108 An Evaluation of Blackberry Harvest Sanitation and the Ability of Foodborne Pathogens to Survive in Blackberry Products 1. Introduction 1.1 Production Blackberries belong to the genus Rubus, subgenus Rubus, and are an important agricultural commodity in Oregon (Hummer 2010). The United States is the largest producer of blackberries in the world, with 65% of the United States production occurring in Oregon in 2005 (Strik and Others 2007). Oregon experienced a 25% increase in blackberry production between 1995 and 2005, and a 6% increase between 2005 and 2011, a trend that is expected to continue (Strik and Others 2007; USDA 2012). Oregon is unique in that the majority of cultivated blackberries are trailing types, which are typically machine harvested. Most states and growing regions predominantly cultivate erect and semierect cultivars. Trailing types typically and with exception, do not produce fruit that is firm enough to withstand extensive shipping and handling to be used for fresh market. Blackberries that are machine harvested are typically destined for further processing into products such as individually quick frozen (IQF) berries, purees, jams, jellies, and even wine (Strik and Others 2007). More than 95% of Oregon blackberries are destined for processing (Strik and Others 2007). In Oregon, the predominant trailing cultivar is ‘Marion’ and accounted for 51% of harvested blackberries in 2011 (USDA 2012). ‘Marion’ is known for its desirable sensory qualities 2 for processing (aroma, acid, and sugar profile) (Strik and Others 2007; Du and Others 2010). Another trailing cultivar that has gained popularity in Oregon is ‘Black Diamond’. ‘Black Diamond’ has the added benefit of being thornless and is suitable for processed products as well as fresh market due to its firmness. This cultivar may be mechanically or hand-harvested (Strik and Others 2007; Du and Others 2010). The trailing cultivar ‘Obsidian’ is mainly grown for hand-harvested fresh market (Finn and Others 2005). ‘Triple Crown’ is also popular in Oregon and is a semierect cultivar. It is hand-harvested, which is typical for erect and semierect types (Strik and Others 2007). Trailing types are harvested between June and August, with erect and semierect types extending into October, depending on cultivar (Strik and Others 2007; Finn and Strik 2008). 1.2 Consumption and Health Benefits Consumption of Rubus fruit, stems, and leaves for food and pharmacological purposes is believed to have begun approximately 10,000 years ago (Hummer 2010). In Oregon, evidence of Rubus consumption can be dated back to 8000 BCE as determined by carbon dating of materials found at Newberry Crater in Bend, OR (Hummer 2010). Ancient Greeks and Romans used nonedible portions of Rubus plants for everything from hair dye to relieving stomach aches. An interesting record of Hippocrates’ writings suggest using blackberry leaves soaked in wine to apply to wounds for antiseptic purposes, a property later understood to be attributed to their tannin content (Hummer 2010). Native populations of North America used Rubus for many ailments related to 3 female reproductive function, including childbirth and menstrual cramps (Hummer 2010). In modern times, blackberries still have much to offer human health. Obesity is understood to be an epidemic in the United States. Fortunately, rates of obesity among American adults appear to have reached a plateau, with obese men comprising 35.5% of the adult population and obese women, 35.8% (Flegal and Others 2012). Obesity is associated with metabolic syndrome which is comprised of a set of risk factors that increase an individual’s likelihood of developing chronic diseases such as diabetes and cardiovascular disease (Gropper and Others 2009). One strategy to help combat obesity in the United States is to increase overall consumption of fruits and vegetables. Healthy People is a program under the Department of Health and Human Services. A primary goal for the Healthy People 2010 objective period was to increase the consumption of fruits and vegetables among Americans. Specifically, the goal was to increase the percentage of individuals over the age of 2 years that consume at least 2 servings of fruit a day to 75% and at least 3 servings a day to 50% (CDC 2010). Figures reported in 2009 showed that the goal was far from being reached with only 32.5% of adults consuming at least 2 servings of fruit daily, a significant decline from 2000, and 26.3% consuming at least 3 servings of vegetables daily (CDC 2010). Figures for Oregon were slightly better with 33% consuming at least 2 servings of fruit daily and 30.5% consuming at least 3 servings of vegetables daily (CDC 2010). To try to improve consumption of fruits and vegetables in the United States, the Centers for Disease 4 Control and Prevention (CDC) has released a guidance document that outlines a 10 point strategy to increase consumption. The overall approach to the strategy is to increase availability and visibility of fruits and vegetables while decreasing cost barriers and increasing consumer education about where their food is coming from. The CDC feels that this can be achieved through such practices as increasing farmers markets, expanding community agriculture programs, and encouraging the availability of fresh produce in markets that tend to not provide as much choice (CDC 2011). Blackberries could serve to help increase overall consumption of fruit, especially when considering the portability and convenience of many blackberry products: for example, fresh, frozen, and freeze dried fruit and blackberry juice. Blackberries also have pleasant sensory properties that make them attractive to consumers across age categories (Du and Others 2010). Nutritionally, they are low in calories, a good source of fiber, and contain vitamins and minerals (USDA Nutrient Database). Many components of blackberries could assist with weight management. Blackberries contain pectin, a soluble fiber. Consumption of pectin has been associated with increased satiety, which may reduce energy overconsumption (Perrigue and Others 2010). Soluble fiber has also been associated with a reduction in blood lipids, which reduces the risk for developing cardiovascular disease (Jenkins and Others 2002; Gropper and Others 2009). Aside from weight loss and management, soluble fiber can be considered a prebiotic, since it is fermentable in the gut, promoting healthy intestinal flora (Gropper and Others 2009). 5 Blackberries are also known to be high in anthocyanin content and antioxidant capacity (Puupponen-Pimia and Others 2005; Tsuda 2012). Consumption of anthocyanins has been demonstrated to assist with obesity and diabetes prevention and or control (Tsuda 2012). Cyanidin-3-glucoside (C3G) is an anthocyanin found in blackberries. Consumption of this chemical has been shown to decrease body fat accumulation in mice even when high fat meals were consumed. The mechanism proposed involved a decrease in lipid synthesis in the liver and white adipose tissues (Tsuda 2012). Cyanidin-3-glucoside was also found to upregulate the expression of adiponectin, which is associated with increased insulin sensitivity (Tschriter 2003; Tsuda 2012). Metabolic syndrome is also associated with increased inflammation, and anthocyanins were associated with the reduction of the inflammatory markers, tumor necrosis factor-α and monocyte chemotactic protein-1 (Sasaki and Others 2007; Tsuda 2012). Gallic acid is a metabolite of anthocyanins and is a powerful antioxidant (Yao and Others 2004). Antioxidants can scavenge free radicals and prevent damage to proteins, lipids, and DNA within the human body. Gallic acid is present in blackberries, but is also a byproduct of anthocyanin metabolism by microorganisms in the human gastrointestinal tract (Aura and Others 2005; Kempler and Humpf 2005). Blackberries can be a healthy addition to the diet considering the numerous ways that they can positively impact human health. 6 1.3 Potential microbial Risks To our knowledge, blackberries have never been implicated in a food safety incident; however microbial safety risks may exist. While chemical and physical hazards are always a possibility (e.g., improperly applied pesticides, thorns), by and large, the most important potential hazards are biological in nature. Sources of microbial contamination could include, but are not limited to: birds, insects, and other animals in the field, microorganisms in soil, environmental molds, contaminated irrigation water, and humans practicing poor hygiene. Machine harvested fruit has less human contact than hand-harvested fruit. However, the impact of proper sanitation of mechanical harvesters is unknown. Additionally, it is possible for the harvester to disturb soil resulting in aerosols, an issue if the soil were contaminated with pathogenic microorganisms. This would be of particular concern when using improperly composted manure in the production system, as it has been found to be able to harbor E. coli for extended periods of time (Beuchat 2002). Fruit that is destined for the fresh market is hand harvested. The safety of this fruit depends on the hygiene practices of the workers. Hand-harvested fruit is packed directly into the plastic clamshell containers that are sold in fresh markets. The fruit does not undergo any washing or microbial decontamination step before reaching the consumer. The clamshells are handled in a way to prevent them from becoming 7 contaminated, using boxes on elevated carts to store them so that they do not touch the ground (Strik and Others 2007). Additionally, fruit that is visibly moldy or in contact with the ground is not harvested (personal observations). Safety becomes an even larger concern when considering that during the offseason, blackberries for fresh market and frozen use are often imported to the U.S. from Mexico and Guatemala (Strik and Others 2007). Guatemalan raspberries (genus, Rubus) were found to be the source of several Cyclosporiasis outbreaks, eventually leading to them having a Detention Without Physical Examination (DWPE) Import Alert placed on them (Herwaldt and Others 1997; FDA 2012). This has resulted in Guatemalan raspberries being prohibited from import during the months of March-August every year (FDA 2012). The DWPE only applies to raspberries; blackberries from Guatemala are allowed to be imported. Frozen raspberries have also been implicated in hepatitis A and norovirus outbreaks (Falkenhorst and Others 2005; Reid and Robinson 1987). At the time of this writing, frozen berries are being implicated in a hepatitis A outbreak that is affecting Denmark, Norway, Sweden, and Finland. At this time, the type of berry and origin are unknown (Gillesberg Lassen 2013). The same strain of hepatitis A has surfaced in an outbreak currently affecting the United States. Again, a frozen berry blend is believed to be the source with the investigation focusing on imported pomegranate seeds that were part of that blend (CDC 2013; Terry 2013). Although not in the Rubus genus, Strawberries (genus Fragaria) are another berry that has been associated with foodborne illness. They were found to be the vehicle for a 2011 8 outbreak of E. coli O157:H7 in Oregon that left one person dead and several more ill: an outbreak later found to be due to deer feces being present in the strawberry fields (FDA 2011; Stone 2011; Terry 2011). Raspberries and blackberries have a similar anatomy. They are comprised of small structures called drupelets that are held together by small hairs that intertwine (Bowling 2000). Both have what is called a receptacle, where the fruit is attached to the plant. Blackberries detach above this and are harvested with the receptacle still in place, which is seen as the white center when looking at the top of a blackberry. Raspberries leave the receptacle behind when harvested, which leaves a hollow center in the fruit (Bowling 2000). The anatomy of the blackberry could potentially give microorganisms of health concern the ability to contaminate and survive on fruit, even if later washing was implemented. The berry skin may not be an ideal location for microorganisms to adhere due its hydrophobic nature; however, the many crevices that exist where drupelets meet, and the receptacle, may provide niches for microorganisms to survive (Bowling 2000). This would be a concern largely for fresh market blackberries, but also exists for the minimally processed IQF blackberries, since many microorganisms can survive freezing. Other blackberry products may not be as susceptible due to the processing method. Puree is often pasteurized, and then frozen, and juice is required to be pasteurized before reaching the consumer. Jams and jellies are heated to an extent that would kill any vegetative bacterial cells. The hostile environment of fermentation 9 during the berry wine making process would be unfavorable to bacterial pathogens, particularly when coupled with the dominance of yeast in the system. The concern with these further processed products is the potential for pathogenic bacteria to be able to survive if post processing contamination occurred. There is evidence that frozen purees and juice concentrates from various fruits can support the survival of E. coli O157:H7, Salmonella spp., and Listeria monocytogenes for at least 12 weeks (Oyarzabal and others 2003). Additionally, E. coli O157:H7, Salmonella spp, and Listeria innocua were able to survive on the surface of frozen strawberries and in strawberry juice over various periods of storage time (Duan and Zhao 2009; Knudsen and Others 2001). Aside from bacterial contamination, blackberries, like other agricultural products, have an opportunistic microflora that will spoil harvested fruit thus, limiting shelf-life. The naturally occurring microflora largely consists of yeasts and molds and will cause spoilage over time. Many fungal species can survive well in the low pH environment of blackberries and consume the organic acids present, which can lead to an increase in the pH of their environment (Tournas and Katsoudas 2005). Depending on the rate at which that occurred, it could be possible for the pH to rise enough to allow some of the more acid tolerant bacterial pathogens to be able to perhaps survive (e.g., E. coli and Salmonella spp.). In retail samples taken from the Washington, D.C. metro area, 100% of blackberries had some sort of fungal population with 78% containing Botrytis cinerea, 33% containing Cladosporium, 22% Fusarium, 22% Penicillin, and 11% Rhizopus (Tournas and Katsoudas 2005). 10 1.4 Potential Antimicrobial Properties Blackberries and blackberry products have many components that may have various degrees of antimicrobial activity. Blackberries naturally have a low pH that ranges from 3.0 to 4.2 (Beuchat 1987). The organic acids present in blackberries are predominantly citric and malic acids. These organic acids can exist in a variety of ratios, depending on cultivar (Fan-Chiang 1999). Organic acids exist in their undissociated form at low pH, which allows them to permeate the plasma membrane of microorganisms (Brul and Coote 1999). Once inside the cell, the organic acids can then dissociate and cause a buildup of protons, eventually becoming toxic to the microorganism (Brul and Coote 1999). Essential oils have been found to be effective against some microorganisms. For example, geraniol, found in blackberries (Du and Others 2010), has been shown to have antimicrobial activity against Salmonella enterica, E. coli O157:H7, and L. innocua (Friedman and Others 2004; Raybaudi-Massilia and Others 2006). Blackberries are a rich source of phenolic compounds including phenolic acids, anthocyanins, and ellagitannins (Puupponen-Pimia and Others 2001; Ruyi and Others 2010). Phenolic compounds may also contribute to antimicrobial activity. Phenolic acids have been demonstrated to be effective against Gram-negative bacteria (Puupponen-Pimia and Others 2001). Some of the phenolic acids and flavonoid compounds found in blackberries include: gallic acid, caffeic acid, coumaric acid, ferulic 11 acid, ellagic acid, catechin, quercetin, and myricetin (Sellappan and Others 2002; Bilyk and Sapers 1986). While tannins may not directly act against microorganisms, they may act indirectly by binding substances needed for their survival such as nutrients, and interfering with microbial extracellular enzyme functions (Puupponen-Pimia and Others 2005). Nohynek and Others (2006) found that extracts from berries in the genus Rubus, cloudberry and raspberry, were able to permeabilize and in some cases disintegrate the outer membrane of Gram-negative bacteria. They attributed this to a synergistic effect of pH and phenolic compounds, noting that gallic acid appeared to have the greatest effect which they believed was due to its ability to chelate divalent cations from the membrane, destabilizing it (Nohynek and Others 2006). This trait is also shared by citric acid (Brul and Coote 1999). In addition, the extracts were found to have an inhibitory effect against several Gram-positive microorganisms, including Staphylococcus aureus. Various wines, and even their unfermented juices, have been demonstrated to have bactericidal properties. Trials with chardonnay juice resulted in bacterial populations of E. coli O157:H7 and Salmonella Typhimurium being reduced to undetectable levels between 3-12 days, and the corresponding wine between 10-57 minutes; pinot noir juice between 10-16 days, and 10-60 minutes in the wine (Just and Daeschel 2003). Another study with unknown grape varieties found that white and red wines resulted in the reduction of E. coli O157:H7 and Salmonella Enteritidis to undetectable levels within 30 minutes (Sugita-Konishi and Others 2001). Interestingly, they did not associate the ethanol content of the wine with the lethality observed due 12 to a solution of 14% ethanol in phosphate-buffered saline not resulting in any reduction in the bacterial populations over a 60 minute period. That conclusion may have neglected to account for the synergistic effect of ethanol, organic acids, and phenolic compounds acting within the same system. Ethanol is known to have a solubilizing effect on the membranes of bacteria, which may allow for easier permealization of other constituents that are toxic to the bacterial cell (Willey and Others 2008). Blackberries are harvested with a soluble solid content far below what is standard for wine grapes (~10-11 °Brix versus 24°Brix) (Du and Others 2010; Zoecklein and Others 1990). Blackberry wines would naturally result in a lower ethanol content than grape wines due to the reduced sugar content unless supplemented. The effect on lethality that this would have in a blackberry wine fermented without sugar supplementation has not, to our knowledge at this time, been previously investigated. While the ethanol content of blackberry wines would be lower, the pH would not be dissimilar, yet the phenolic content would vary widely, depending on fruit type and cultivar. 13 2. An Evaluation of Blackberry Harvest Sanitation and the Ability of Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus to Survive on the Surface of Fresh and Frozen Blackberry Fruit Melissa M. Sales and Mark A. Daeschel Oregon State University Department of Food Science and Technology, Corvallis OR 97331 To be submitted to: Journal of Food Science Institute of Food Technologists 525 W. Van Buren Ste 1000 Chicago Ill 60607 14 2.1 Abstract Blackberries, genus Rubus, are an important Oregon agricultural commodity. In their fresh and processed forms, they offer many health benefits and may be able to help Americans better achieve fruit consumption recommendations because of convenience and pleasant sensory qualities. However, the susceptibility of blackberry products to contamination with bacterial pathogens of human health concern is unknown. Blackberries have never directly been implicated in a food safety incident; however, raspberries, also in the Rubus genus, have been the vehicle for hepatitis A, norovirus, and Cyclospora cayetanensis outbreaks. Furthermore, strawberries were recently the source of an Escherichia coli O157:H7 outbreak in Oregon. To better understand the potential for microbial pathogen contamination and the ability of these organisms to survive or grow in blackberry products, several studies were conducted. Fresh berries from the ‘Obsidian’ and ‘Triple Crown’ cultivars were evaluated at different harvest periods for the aerobic plate count, coliforms, yeasts, and molds to establish a baseline microbial population. Environmental samples were taken from a clean mechanical harvester and then from the same harvester that had been intentionally left soiled with berry harvest debris to determine the impact of harvester sanitation. Samples from ‘Marion’ and ‘Black Diamond’ cultivars were hand harvested and evaluated for E. coli O157:H7 and Salmonella spp. by rapid detection methods via the NEOGEN® Reveal® 2.0 systems. Fresh, wild ‘Himalaya’ blackberries and frozen blackberries from the ‘Triple Crown’ cultivar were spot inoculated with E. coli O157:H7, 15 Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus to determine the ability of these microorganisms to survive on the berry surface. ‘Himalaya’ samples were stored for 3 days at ambient temperatures and ‘Triple Crown’ for 6 months at -23.3°C. Aerobic plate counts (APC) for ‘Obsidian’ and ‘Triple Crown’ cultivars ranged from 3.52-4.62 log CFU/g of berry with the late harvest ‘Triple Crown’ samples having a significantly higher APC than early harvest samples (p = 0.005). Yeasts and molds ranged from 3.01-4.73 log CFU/g berry with both cultivars having significantly higher counts at later harvest times (p = 0.048 ‘Obsidian’; p < 0.001 ‘Triple Crown’). Coliforms were detected in ‘Obsidian’ mid-harvest and ‘Triple Crown’ early-harvest samples at 2.10 and 1.40 log CFU/g of berry, respectively. The overall aerobic plate counts measured from the mechanical harvester were not affected by machine cleanliness. Escherichia coli O157:H7 and Salmonella spp. were not detected using rapid detection methods in evaluated ‘Marion’ and ‘Black Diamond’ samples. Escherichia coli O157:H7 was not detectable in fresh or frozen inoculated samples. Salmonella Typhimurium was detected in 2 frozen samples with 2.95 and 3.21 log reductions. Listeria monocytogenes was only detected in frozen samples and experienced log reductions ≥ 2.42. Staphylococcus aureus was detectable on every fresh and frozen berry inoculated with log reductions ranging from 0.67 to 3.48, the greatest reductions occurring in fresh samples. 16 The overall results suggest that blackberries are not an ideal environment for E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus to grow. However, these microorganisms may be able to survive depending on the type of blackberry product and its subsequent storage. 2.2 Introduction Blackberries, genus Rubus, are an important agricultural commodity in Oregon. In 2011, 24,212,760 kg of cultivated blackberries were produced in Oregon and valued at over 43 million USD (USDA 2012). There are three types of blackberries plants: trailing, erect, and semierect. Oregon is unique in that the majority of cultivated blackberries in this state are trailing cultivars, most notably ‘Marion’, whereas many other growing regions cultivate erect and semierect types (Strik and Others 2007; USDA 2012). Trailing cultivars are typically machine harvested for processed markets, while erect and semierect cultivars are hand-harvested for fresh market. There are exceptions, and the popular ‘Black Diamond’ cultivar is an example. ‘Black Diamond’ is a trailing cultivar, but has the benefit of being thornless and produces fruit firm enough to be able to withstand shipping and handling required for fresh market. It can be mechanically or hand-harvested depending on its intended use (Finn and Others 2005; Strik and Others 2007). Machine harvested fruit is most often destined for further processing into individually quick frozen (IQF) berries, jams, purees, juices, and even wines (Strik and Others 2007). The trailing cultivar ‘Obsidian’ is hand-harvested for fresh market (Finn and Others 2005). ‘Triple Crown’ is a popular semierect cultivar in 17 Oregon and is hand harvested for fresh market (Finn and Strik 2008; Strik and Others 2007). ‘Himalaya’ is considered an invasive species, but is still popular for noncommercial harvesting in Oregon (Finn and Strik 2008). Table 2.1 Cultivar Information Cultivar ‘Marion’ ‘Black Diamond’ ‘Obsidian’ ‘Triple Crown’ ‘Himalaya’ Type Trailing Trailing Trailing Semierect N/A (similar to semierect) Farming Method Certified Organic Certified Organic Certified Organic Certified Organic Wild Blackberries are harvested from June through October, depending on the cultivar and type, with each cultivar having a fruiting season of 3-6 weeks (Finn and Strik 2008; Strik and Others 2007). When considering the value of the Oregon blackberry harvest combined with the short fruiting season, the economic impact of a food safety recall could devastate the industry. The season is of such short duration that economic recovery following a recall would be very unlikely. Blackberries have never been implicated in a food safety incident; however, other berry fruits have. Frozen raspberries, also in the Rubus genus, have been the source of Cyclospora cayetanensis, norovirus, and hepatitis A outbreaks (Ho and Others 2002; Reid and Robinson 1987; Sarvikivi and Others 2012). The anatomy of raspberries is similar enough to blackberries to warrant concern of blackberries being susceptible to similar contamination. Currently, frozen berries are believed to be the source of a hepatitis A outbreak in Denmark, Norway, Sweden, and Finland (Gillesberg and Lassen 18 2013). The same strain of hepatitis A has surfaced in an outbreak affecting the United States, again a frozen berry blend believed to be the source with the investigation focusing on imported pomegranate seeds that were included in the blend (CDC 2013; Terry 2013). Although not in the Rubus genus, fresh strawberries (genus Fragaria) were the source of an outbreak of Escherichia coli O157:H7 in Oregon that left one dead and several others ill, demonstrating that other berry fruits are vulnerable to contamination as well (FDA 2011; Terry 2011). The outbreaks associated with raspberries and other berry blends have in common that humans are the reservoir for hepatitis A, Cyclospora cayetanensis, and norovirus. This suggests that berries may be susceptible to contamination with other causal agents of foodborne illness that humans are known to be carriers of. These could include Staphylococcus aureus, pathogenic strains of Escherichia coli, and Salmonella spp. Thus, poor hygiene of workers involved with harvesting and/or handling fruit could result in contamination of blackberries. Other sources of contamination are possible. Birds are known reservoirs of Salmonella. Flies have been demonstrated to be able to transmit E. coli O157:H7 to damaged apples (Janisiewicz and Others 1999). Deer were determined to be the source of the E. coli O157:H7 outbreak associated with strawberries (Stone 2011; Terry 2011). Additionally, contaminated soil or irrigation water, and perhaps even the harvesting equipment could be sources of contamination. 19 Blackberries are a portable, convenient fruit with a pleasant aroma and flavor that could encourage individuals in the United States to consume the recommended daily servings of fruits (Du and Others 2010). Nationally, only 32.5% of Americans consume at least two servings of fruit daily (CDC 2010). Increasing fruit and vegetable consumption as a strategy to combat the obesity epidemic is a goal of the Centers for Disease Control (CDC 2011). These goals increase the need to understand how foodborne pathogens behave in various fruit and vegetable environments to avoid increased consumption having unintended consequences. Understanding how certain microorganisms behave in the blackberry environment will help the blackberry industry better employ prevention strategies, understand the risk involved with their product, and to be prepared to quickly respond in the event of any contamination. Blackberries are known to naturally have a diverse microflora of yeasts and molds on their surface (Tournas and Katsoudas 2005); however, not much information that quantifies the microflora is available. The relationship that these yeasts and molds may have with bacterial pathogens, if present, is not well understood. It has been suggested that they may inhibit pathogenic species by dominating the environment or may even encourage growth by making nutrients available and altering the surrounding pH (Beuchat 2002; Tournas and Katsoudas 2005). Blackberries have chemical constituents that could affect the ability of foodborne pathogens to survive. Organic acids are abundant in blackberries, resulting in the fruit having a low pH; conditions known to prevent growth and cause bacterial 20 death in many species (Beuchat 1987; Brul and Coote 1999; Jay and Others 2005). Blackberries are also a rich source of phenolic compounds, many of which have been found to be bactericidal. Phenolic acids have been shown to be effective against Gramnegative bacteria and tannins are known to bind substances the bacterial cells need to survive (Puupponen-Pimia and Others 2005, 2007). Furthermore, extracts from other berries in the Rubus genus have been found to be antagonistic toward Gram-negative and Gram-positive bacteria (Nohynek and Others 2006). To better understand the microflora associated with blackberries and how pathogenic bacteria may behave in whole berries, three primary goals for this study were established: 1) establish quantifiable information about the microflora populations on blackberries; 2) evaluate the sanitation of mechanical harvesters; and 3) evaluate the ability of foodborne pathogens to survive on fresh and frozen blackberries. 2.3 Materials and Methods 2.3.1 Fresh Field Samples Samples of ‘Obsidian’ and ‘Triple Crown’ blackberries at their early, mid, mid/late, or late harvest periods were obtained from Riverbend Organic Farms in Jefferson, OR and evaluated for the aerobic plate count (APC), yeast and molds, and coliforms. Samples arrived in plastic clamshell containers and were analyzed the same day as harvest. Two clamshells were obtained for each cultivar at each harvest point evaluated. A 50 g sample taken from each clamshell was homogenized at 200 RPM for 2 minutes (Stomacher® 400 Circulator; Seward Laboratory). Homogenized samples were 21 immediately serially diluted in sterile Butterfield’s phosphate buffer (referred to as phosphate buffer for simplicity) and plated on Plate Count Agar (PCA;Difco), Dichloran Rose Bengal Chloramphenicol Agar (DRBC; EMD), and Violet Red Bile Agar (VRB; ColeParmer Instrument Company). Plate Count Agar plates were incubated for 48h at 30°C, DRBC plates for 48-72h depending on growth at 30°C, and VRB plates for 24h at 35°C. 2.3.2 Direct Pathogen Testing Early, mid, and late harvest samples of ‘Marion’ and ‘Black Diamond’ blackberries were collected by hand-harvesting at the North Willamette Research and Extension Center (NWREC) in Aurora, OR. Berries were separated by cultivar and placed in plastic bags. They were transported under refrigeration to Oregon State University and evaluated the same day. Samples were evaluated for Salmonella spp. and E. coli O157:H7 using modified protocols for the NEOGEN® Reveal® 2.0 Salmonella and NEOGEN® Reveal® 2.0 E. coli O157:H7 Complete Systems for rapid detection. From each cultivar, 25 g samples were placed in a sterile 500 ml media bottle and covered with 100 ml of phosphate buffer. This was conducted in duplicate for each cultivar. The berries were gently agitated in the solution at room temperature. For Salmonella testing, one bottle of REVIVE® recovery medium was added to a sterile 500 ml media bottle and mixed with 200 ml of sterile deionized (DI) water at 4243°C. From the berry sample, 25 ml of phosphate buffer was removed, added to the REVIVE® mixture and then incubated for 4 h at 36°C. The contents of one bottle of provided 2xRV selective media was added to 200 ml of sterile DI water at 37°C and then 22 held at 42°C until ready to use. After the solution containing the sample completed its 4 h incubation, the 2xRV solution was added to it and then incubated at 42°C for an additional 24 h. Using the provided sterile dropper, 200 µl were transferred to a sample cup. The test strip was inserted and allowed to stand for 15 m at room temperature before reading. For E. coli testing, one bottle of Reveal® 2.0 E. coli O157:H7 media was placed in a sterile 500 ml media bottle and mixed with 325 ml of sterile DI water at 42°C. From the berry sample, 65 ml of the phosphate buffer was removed, added to the media, and incubated at 42°C for 20 h. After incubation, 200 µl was transferred to the test cup provided. A drop of provided promoter agent was added and then incubated for an additional 15 m. The test strip was placed in the sample cup while it was still in the incubator and was read after 15 m. All media and reagents used were included in the test kits and experiments were conducted in duplicate. All incubation periods occurred with media bottles loosely lidded to allow for air exchange. Efficacy of the NEOGEN® Reveal® systems was verified using pure culture spiked berry samples and negative controls. 2.3.3 Mechanical Harvester Sterile swabs were used to take 8 environmental samples from a clean mechanical harvester (over-the-row Littau Harvester; Stayton,OR) at the NWREC just prior to harvesting ‘Marion’ blackberries. Locations sampled were photographed for future reference and can be viewed in Appendix II. Swabs were moistened in phosphate 23 buffer prior to location sampling. Once sampled, the swabs were agitated in culture tubes containing 4 ml of phosphate buffer. Samples from the tubes were serially diluted and plated on PCA. Plates were incubated for 48 h at 30°C. The mechanical harvester remained intentionally unwashed after the ‘Marion’ harvest and post-harvest environmental samples were taken 48 h after the initial samples. The same 8 locations were sampled. Sample handling and plating occurred in the same manner as the initial sampling. 2.3.4 Whole Berry Inoculation 2.3.4.1 Culture Preparation Cultures of Escherichia coli O157:H7 (ATCC 43894), Salmonella Typhimurium (ATCC 14028), Listeria monocytogenes (Scott A), and Staphylococcus aureus (general food isolate, 648 in OSU Culture Collection) were used for spot inoculation studies. All cultures used were from the culture collection at Oregon State University, Department of Food Science and Technology. Cultures maintained in Trypticase Soy Broth (TSB) were transferred to fresh TSB and incubated for 24h at 35°C (BBL™ Trypticase Soy Broth™, BD). One hundred microliters from each were again transferred to fresh TSB and incubated for 18 h at the same temperature. These cultures were then serially diluted in phosphate buffer and used for inoculation. Enumeration was determined by serial dilution on Trypticase Soy Agar (TSA) (Bacto™ Agar, BD; BBL™ Trypticase Soy Broth™, BD). 24 2.3.4.2 Fresh Berry Samples ‘Himalaya’ blackberries were obtained from Bald Hill Vineyard in Corvallis, OR and kept at 8°C. Inoculation occurred the day following harvest. Individual berries were placed on a sterile cap, which were then placed in a Nalgene tray. Berries were then inoculated with 10 µl aliquots of a single bacterial strain in 5 locations for a total of 50 µl per berry (5.18-6.47 log CFU/g of berry). Inoculated berries were allowed to dry overnight under a biosafety hood. After drying, the tray containing the berries was moved to an incubator held at room temperature and rotated several times per day for 3 d. Each berry was then placed in a beaker, had 10 ml of phosphate buffer added to it and then gently agitated. This ‘rinse’ solution was then serially diluted and plated on TSA. All plates were incubated at 35°C for a period of 6 h to allow injured cells an opportunity to recover (Mahmoud and Others 2010). Using the weight of the berry sample, enough phosphate buffer was added to the berry/phosphate sample to equal a 1:10 dilution and then homogenized at 230 RPM for 30 s (Stomacher®400 Circulator, Seward). The resulting mixture was serially diluted and plated on TSA, allowing for the same recovery period as described above. After the recovery period, a layer of appropriate selective media was placed over the TSA: Sorbitol MacConkey Agar(SMAC; Difco) for E. coli O157:H7; Xylose Lysine Deoxycholate Agar (XLD; Difco) for Salmonella Typhimurium; Oxford Listeria Agar Base with Oxford Listeria Selective Supplement (EMB 25 and Sigma Aldrich) for L. monocytogenes; and Mannitol Salt Agar (MSA; BBL) for S. aureus. 2.3.4.3 Frozen Berry Samples ‘Triple Crown’ blackberries were hand harvested from Riverbend Organic Farms and kept at 8°C. Inoculation occurred the day following harvest. Individual berries were placed in sterile glass jars and inoculated with a single bacterial strain (3.54-4.55 log CFU/g of berry). Berries were inoculated with 5 µl aliquots in 10 locations for a total of 50 µl per berry. Berries were allowed to remain under a biosafety hood until visibly dry, covered with sterilized foil, and frozen at -23.3°C for 6 months. For evaluation, each berry was removed from the freezer just prior to analysis. Evaluation occurred in the same manner as described above for fresh berry evaluation with the following modification: initial rinse with 10 ml phosphate buffer occurred in the glass jar containing the berry, after which the berry was gently removed with forceps and placed into a filtered stomacher bag. 2.3.5 Data Analysis All data were analyzed using Microsoft Excel with the exception of analyses of the aerobic plate count, yeasts and molds, and mechanical harvester aerobic plate counts, which were evaluated by hypothesis tests with Statgraphics Centurion. 2.4 Results and Discussion 2.4.1 Fresh Field Data The aerobic plate counts (APC) for ‘Obsidian’ and ‘Triple Crown’ cultivars at their early, mid, mid/late, or late harvest periods ranged from 3.52 to 4.62 log CFU/g of berry 26 (Figure 2.1). Counts were higher for both cultivars at their later harvest time, with ‘Triple Crown’ mid/late harvest having significantly higher APC (p = 0.005). Figure 2.2 shows that yeasts and molds ranged from 3.01 to 4.73 log CFU/g of berry, with ‘Obsidian’ late harvest having the highest values. Later harvests for both cultivars were observed to have significantly higher yeast and mold counts than earlier harvests (p = 0.048 ‘Obsidian’; p < 0.001 ‘Triple Crown’). Caution should be taken when interpreting these findings considering that the summer of 2011, when these samples were taken, experienced an exceptional amount of rain (Oregon Climate Service 2011). This could have resulted in lower values than normal if microorganisms were being washed off fruit by the rain, or higher values if the increased moisture was providing better growth/survival conditions. Published values for the aerobic plate count, yeasts, and molds for blackberries were not found in a search of the literature; however, our data were consistent with values obtained from fresh strawberry rinse water (Jensen and others 2012). Coliforms were detected in ‘Obsidian’ mid harvest and ‘Triple Crown’ early harvest samples at 2.10 and 1.40 log CFU/g of berry, respectively (Figure 2.3). The detection limit for the experimental design was 0.70 log CFU/g. Follow up tests were not conducted to determine if these coliforms were fecal in origin. 27 APC Log CFU/g Figure 2.1 Aerobic Plate Count at Various Harvest Times for 'Obsidian' and 'Triple Crown' Cultivars. Bars indicate the range (high and low values); weeks are for 2011. 5 4.5 4 3.5 3 2.5 2 1.5 1 0.5 0 Obsidian Mid Obsidian Late Triple Crown Early Triple Crown Harvest: Week 29 Harvest: Week 30 Harvest: Week 34 Mid/Late Harvest: Week 35 Figure 2.2 Yeasts and Molds at Various Harvest Times for 'Obsidian' and 'Triple Crown' Cultivars. Bars indicate the range (high and low values); weeks are for 2011. Yeasts and Molds Log CFU/g 5 4.5 4 3.5 3 2.5 2 1.5 1 0.5 0 Obsidian Mid Obsidian Late Triple Crown Early Triple Crown Harvest: Week 29 Harvest: Week 30 Harvest: Week 34 Mid/Late Harvest: Week 35 28 Figure 2.3 Coliforms at Various Harvest Times for 'Obsidian' and 'Triple Crown' Cultivars. Dotted line indicates the lower limit for the detection of coliforms; Bars indicate the range (high and low values); weeks are for 2011. 2.5 Coliforms Log CFU/g 2 1.5 1 <0.70 Log CFU/g <0.70 Log CFU/g 0.5 0 Obsidian Mid Harvest: Week 29 Obsidian Late Harvest: Week 30 Triple Crown Early Harvest: Week 34 Triple Crown Mid/Late Harvest: Week 35 2.4.2 Direct Pathogen Testing The results for the direct testing of E. coli O157:H7 and Salmonella spp. are shown in Table 2.2. Neither pathogen was detected in any of the samples evaluated. Table 2.2 Detection of E. coli O157:H7 and Salmonella spp. in ‘Marion’ and ‘Black Diamond’ Cultivars using rapid detection methods Early 7/9/12 ‘Marion’ E. coli Salmonella Rep 1 Rep 2 Rep 1 Rep 2 Negative Negative Negative Negative ‘Black Diamond’ Negative Negative Negative Negative Mid 7/12/12 ‘Marion’ Negative Negative Negative Negative ‘Black Diamond’ Negative Negative Negative Negative Late 7/19/12 ‘Marion’ Negative Negative Negative Negative ‘Black Diamond’ Negative Negative Negative Negative 29 2.4.3 Mechanical Harvester Microbial populations for individual sample locations on the mechanical harvester varied substantially (Figure 2.4). Little change occurred pre- and post-harvest at locations 2, 5, 6, and 7. Photographs of sampled locations can be viewed in Appendix II. A 2.03 log reduction was observed at location 3 post-harvest. Moderate increases were observed at locations 1, 4, and 8 with location 8 experiencing the largest increase (2.0 log). Figure 2.4 Mechanical Harvester Aerobic Plate Counts: Clean and Unwashed 5 4.5 4 Log CFU/Swab 3.5 3 2.5 Clean 2 48 h After Intentionally Left Unwahsed 1.5 1 0.5 0 Location on Mechanical Harvester When an overall aerobic plate count for the mechanical harvester was determined using all locations sampled, there was not a significant difference in clean 30 and intentionally dirtied values (p = 0.452). These results indicate that the microbial quality of the mechanical harvester does not change 48h post-harvest, even with washing not occurring between sampling periods. This is likely due to the organic acids released from the berries during harvest combined with UV radiation inhibiting growth (Brul and Coote 1999; Rico and Others 2007). 2.4.4 Spot Inoculation Studies 2.4.4.1 Fresh Berry Results Escherichia coli O157:H7, Salmonella Typhimurium, and L. monocytogenes were not detected in the ‘Himalaya’ samples 3 d after inoculation (Tables 2.3-2.5). Staphylococcus aureus was recovered from both inoculated berries, but only in the evaluation of the homogenized samples (Table 2.6). Staphylococcus aureus experienced log reductions of 3.03 and 3.48 in these samples. Table 2.3 ‘Himalaya’ inoculated with E. coli O157:H7, evaluated after 3 d held at ambient temperatures Sample Inoculum per gram of berry Rinse Recovery Homogenized Recovery Berry 1 5.74 Log CFU/g Berry 2 5.69 Log CFU/g <0.70 Log CFU/g < 0.70 Log CFU/g <1.70 Log CFU/g <1.70 Log CFU/g 31 Table 2.4 ‘Himalaya’ inoculated with Salmonella Typhimurium, evaluated after 3 d held at ambient temperatures Sample Inoculum per gram of berry Rinse Recovery Homogenized Recovery Berry 1 5.80 Log CFU/g Berry 2 5.87 Log CFU/g < 0.70 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g <1.70 Log CFU/g Table 2.5 ‘Himalaya’ inoculated with L. monocytogenes, evaluated after 3 d held at ambient temperatures Sample Inoculum per gram of berry Rinse Recovery Homogenized Recovery Berry 1 6.25 Log CFU/g Berry 2 6.47 Log CFU/g < 0.70 Log CFU/g < 0.70 Log CFU/g <1.70 Log CFU/g <1.70 Log CFU/g Table 2.6 ‘Himalaya’ inoculated with S. aureus, evaluated after 3 d held at ambient temperatures Sample Inoculum per gram of berry Rinse Recovery Homogenized Recovery Berry 1 5.33 Log CFU/g Berry 2 5.18 Log CFU/g < 0.70 Log CFU/g < 0.70 Log CFU/g 2.30 Log CFU/g 1.70 Log CFU/g 2.4.4.2 Frozen Berry Results Escherichia coli O157:H7 was not detected in any of the frozen ‘Triple Crown’ samples (Table 2.7). Salmonella Typhimurium was detected in 2 of the 7 inoculated berries, and only in the rinse water with 2.95 and 3.21 log reductions (Table 2.8). It 32 should be noted that one of the berries was evaluated at 3 months to establish to the procedure protocol. Listeria monocytogenes was detected in 3 of the 7 inoculated berries, all 3 in the homogenized samples with recovery also occurring in one of the rinse samples (Table 2.9). Log reductions of L. monocytogenes ranged from 2.42-3.42 when detected. Staphylococcus aureus was detected in all 7 inoculated berries, 4 of the 7 in the rinse water and 5 of the 7 in homogenized samples (Table 2.10). Log reductions of S. aureus ranged from 0.67-3.48. The detection limit for rinse water was 0.70 log CFU/g berry and 1.70 log CFU/g berry for homogenized samples. Table 2.7 Frozen ‘Triple Crown’ inoculated with E. coli O157:H7, evaluated after 6 months stored at -23.3°C Sample Berry 1 Inoculum per gram of berry 4.40 Log CFU/g Rinse Recovery <0.70 Log CFU/g Homogenized Recovery <1.70 Log CFU/g Berry 2 4.50 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 3 4.45 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 4 4.42 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 5 4.34 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 6 4.36 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 7 4.31 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g 33 Table 2.8 Frozen ‘Triple Crown’ inoculated with Salmonella Typhimurium, evaluated after 6 months stored at -23.3°C (*Berry 1 evaluated after 3 months) Sample Rinse Recovery Berry 1* Inoculum per gram of berry 3.95 Log CFU/g 1.00 Log CFU/g Homogenized Recovery <1.70 Log CFU/g Berry 2 3.90 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 3 4.04 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 4 3.96 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 5 3.91 Log CFU/g 0.70 Log CFU/g <1.70 Log CFU/g Berry 6 3.87 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 7 4.00 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Table 2.9 Frozen ‘Triple Crown’ inoculated with L. monocytogenes, evaluated after 6 months stored at -23.3°C Sample Berry 1 Inoculum per gram of berry 4.32 Log CFU/g Rinse Recovery <0.70 Log CFU/g Homogenized Recovery 1.70 Log CFU/g Berry 2 4.42 Log CFU/g 1.00 Log CFU/g 2.00 Log CFU/g Berry 3 4.24 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 4 4.31 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 5 4.55 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g Berry 6 4.24 Log CFU/g <0.70 Log CFU/g 1.70 Log CFU/g Berry 7 4.27 Log CFU/g <0.70 Log CFU/g <1.70 Log CFU/g 34 Table 2.10 Frozen ‘Triple Crown’ inoculated with S. aureus, evaluated after 6 months stored at 23.3°C Sample Berry 1 Inoculum per gram of berry 3.59 Log CFU/g Rinse Recovery <0.70 Log CFU/g Homogenized Recovery 2.18 Log CFU/g Berry 2 3.62 Log CFU/g 0.70 Log CFU/g <1.70 Log CFU/g Berry 3 3.58 Log CFU/g 0.70 Log CFU/g <1.70 Log CFU/g Berry 4 3.56 Log CFU/g 1.00 Log CFU/g 1.70 Log CFU/g Berry 5 3.60 Log CFU/g <0.70 Log CFU/g 2.93 Log CFU/g Berry 6 3.54 Log CFU/g <0.70 Log CFU/g 2.00 Log CFU/g Berry 7 3.63 Log CFU/g <0.70 Log CFU/g 1.70 Log CFU/g These results indicate that the surface of blackberry fruit is not suitable for these bacteria to grow; however, they may survive. Escherichia coli O157:H7 appears to be the least able to survive either on fresh or frozen berry surfaces, whereas S. aureus was the most able to persist. Freezing of the inoculated fruit appears to improve survival, which was to be expected considering that freezing is a method frequently used to preserve microorganisms (Jay and Others 2005). Furthermore, E. coli O157:H7 and Salmonella spp. have been found to be able to survive on the surface of frozen strawberries for at least 30 d (Knudsen and Others 2001). The aqueous nature of the inocula may have also contributed to the minimal survival observed. Blackberry fruit has a waxy surface that protects it from a variety of stresses, including osmotic pressure (Bowling 2000; Shepherd and Griffiths 2006). It was 35 observed during the inoculation procedure that the inoculum would form beads on the hydrophobic berry surface. This may have resulted in some of the bacterial cells experiencing desiccation as the phosphate buffer evaporated, leaving few viable cells in contact with the actual berry. In harvesting/processing settings, fruit would become contaminated by feces, hands, soil, etc. These other sources of contamination may lead to better bacterial survival on the blackberry surface. 2.5 Conclusions The blackberry surface is not an environment that will allow the growth of E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus. The microflora that was observed in fresh blackberry samples may offer some protection by outcompeting/antagonizing bacterial pathogens (Beuchat 2002). Moreover, E. coli O157:H7 was not observed to survive in any fresh and frozen samples within the experimental detection limits. However, the observation that there was survival by some pathogens reinforces the need for sanitary harvesting conditions and handling to prevent the contamination of blackberries that are destined for fresh market or IQF processing. The mechanical harvester used to harvest trailing type blackberries is not likely to be a source of contamination, particularly if it is exposed to sunlight (Rico 2007). Any blackberry residue may actually reduce microbial populations on the harvester by exposure to organic acids; however, these results should not be taken as a suggestion to not wash mechanical harvesters post-harvest. The larger concern lies with the hygiene 36 of workers handling the blackberry fruit. Humans are known reservoirs of S. aureus and can also harbor pathogenic strains of E. coli and Salmonella spp. Furthermore, they are also known reservoirs of Hepatitis A, norovirus, and Cyclospora cayetanensis, all of which have been the cause of foodborne illnesses associated with raspberries indicating that humans can contaminate berries in the Rubus genus (Ho and Others 2002; Reid and Robinson 1987; Sarvikivi and Others 2012). Although E. coli O157:H7 and Salmonella spp. were not detected in directly harvested and tested samples, it is important to consider other non-human sources of contamination. Animals, contaminated soil, or irrigation water could result in contamination with a variety of microorganisms of human concern. These sources can be avoided by establishing and maintaining sanitary growing, harvesting, and handling practices. 37 3. An Evaluation of the Survival of Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus in ‘Marion’ and ‘Black Diamond’ Blackberry Juice and Wine Melissa M. Sales and Mark A. Daeschel Oregon State University Department of Food Science and Technology, Corvallis OR 97331 To be submitted to: Journal of Food Science Institute of Food Technologists 525 W. Van Buren Ste 1000 Chicago Ill 60607 38 3.1 Abstract Blackberries, genus Rubus, are an important Oregon agricultural commodity that is frequently processed into various products. These products include individually quick frozen (IQF) berries, jams, juices, purees, and even wines. However, the susceptibility of blackberry products to contamination with bacterial pathogens of human health concern is unknown. Previous studies and food safety incidents have demonstrated that many pathogenic microorganisms are able to survive in purees, juices, and frozen concentrates made from various fruits. Survival studies were conducted in juices and wines made from ‘Marion’ and ‘Black Diamond’ purees to understand the potential for pathogenic bacteria to survive if post-processing contamination were to occur. Furthermore, the studies were designed to yield information about what chemical constituents of the juices and wines may contribute to antibacterial activity. Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, and Staphylococcus aureus were evaluated for their ability to survive in these products. Growth of microorganisms was not observed in any juice or wine samples. Maximum observed survival times in juices ranged from 12 h for L. monocytogenes to 108 h for Salmonella Typhimurium. Maximum survival times in wines were 40 m for both E. coli O157:H7 and Salmonella Typhimurium, and 80 m for both L. monocytogenes and S. aureus. Adding ethanol to juice samples to equal that of their counterpart wines decreased survival time for all microorganisms evaluated by several hours. Increasing 39 the pH of wines by approximately one unit increased the survival time from minutes to hours, and in some cases, days. These results demonstrate that blackberry juice and wine do not support the growth of E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus. However, these microorganisms may be able to survive for various periods of time depending on the type of blackberry product. Many constituents of blackberries may offer bactericidal activity, with organic acids appearing to have the greatest effect. 3.2 Introduction Blackberries are an important agricultural commodity in Oregon with 65% of the U.S. production occurring in this state (Strik and Others 2007). There are three types of blackberry plants: trailing, erect, and semierect. Oregon is unique in that cultivated blackberries are predominantly trailing types, with the primary cultivar being ‘Marion’, whereas other growing regions typically grow erect and semierect types (Strik and Others 2007; USDA 2010). ‘Black Diamond’ is another popular trailing type in Oregon, but has the added benefit of being thornless and produces firm enough fruit to withstand shipping and handling, resulting in this cultivar being suitable for both mechanical and hand-harvesting (Finn and Strik 2008; Strik and Others 2007). Table 3.1 Cultivar Information Cultivar Type ‘Marion’ Trailing ‘Black Diamond’ Trailing Farming Method Conventional Certified Organic 40 Machine harvested blackberries are most often destined for further processing, whereas hand-harvested fruit is used for fresh market. Machine harvested fruit may be processed into individually quick frozen (IQF) berries, purees, jams, juices, and even wines (Strik and Others 2007). Individually quick frozen berries are minimally processed and could be at risk for contamination. Jams, juices, and some purees undergo a thermal processing procedure that would effectively kill any vegetative pathogenic bacterial cells present. These cells would also not be likely to survive fermentation during the blackberry wine making process. For these fermented and thermally processed products, the concern is whether or not bacterial pathogens of human concern could survive in the event of post-processing contamination. The scope of this study will focus on the ability of foodborne pathogens to survive in processed blackberry juices and wines. There is evidence that frozen purees and juice concentrates from various fruits can support the survival of Escherichia coli O157:H7, Salmonella spp., and Listeria monocytogenes for at least 12 weeks (Oyarzabal and Others 2003). Previous studies using chardonnay juice resulted in bacterial populations of E. coli O157:H7 and Salmonella Typhimurium being reduced to undetectable levels between 3-12 days, and the corresponding wine between 10-57 minutes; pinot noir juice between 10-16 days, and 10-60 minutes in the wine (Just and Daeschel 2003). Another study with unknown grape varieties found that white and red wines resulted in the reduction of E. coli 41 O157:H7 and Salmonella Enteritidis to undetectable levels within 30 minutes (SugitaKonishi and Others 2001). There are several chemical constituents of blackberry juices and wines that may contribute to bactericidal activity. Organic acids are abundant in blackberries, typically as citric and/or malic acids in varying ratios, depending on cultivar (Fan-Chiang 1999). This results in the fruit having a low pH, conditions known to prevent growth and cause cellular death in many bacterial species (Beuchat 1987; Brul and Coote 1999; Jay and Others 2005). Blackberries are also a rich source of phenolic compounds, such as phenolic acids, anthocyanins, and ellagitannins (Puupponen-Pimia and Others 2001; Wu and Others 2010). Phenolic acids have been shown to be effective against Gramnegative bacteria and the tannins bind substances the bacterial cells need to survive (Puupponen-Pimia and Others 2001, 2005). Furthermore, extracts from other berries in the Rubus genus have been found to be effective against Gram-negative and Grampositive bacteria (Nohynek and Others 2006). Ethanol, present in wines, is known to have a solubilizing effect on the membranes of bacteria, which may allow for easier permealization of other constituents that are toxic to the bacterial cell (Willey and Others 2008). The objectives for this study were to evaluate the ability of E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and Staphylococcus aureus to survive in blackberry juices and wines, and to understand which constituents of the juices and wines contribute to antibacterial activity. 42 3.3 Materials and Methods 3.3.1 Juice and Wine Preparation Approximately 34 kg each of ‘Marion’ and ‘Black Diamond’ blackberries were collected for the purpose of making juice and wine. ‘Marion’ fruit was harvested by machine in a single harvest from the North Willamette Research and Extension Center (NWREC) in Aurora, OR. After collection, the fruit was pureed and frozen at -23.8°C for further use. ‘Black Diamond’ blackberries were hand-harvested from Riverbend Organic Farms in Jefferson, OR. Fruit were harvested over the ‘Black Diamond’ fruiting season (July, 2011) and frozen at -23.8°C until 34 kg was accumulated, after which, the berries were thawed and pureed before being frozen again for future use. Purees were thawed and equally divided. Half of each puree was hand pressed through a mesh bag in order to release juice. The juices were then bottled in 187 ml glass bottles, capped with crown caps, and pasteurized in a water bath at 71°C for 25 m. The other half of each puree was placed into 38 L plastic buckets and inoculated with Saccharomyces cerevisiae for the purpose of making wine. After 5 d of fermentation at ambient temperatures, both the liquid and pulp components of the wine were strained through a mesh bag and the filtered liquids were transferred to 11 L carboys for continued fermentation for 5 d. The wine was then racked and bottled into 187 ml glass bottles, crown capped, and pasteurized as described above. Bottles of juice and wine were boxed and kept out of light at room temperature for further use. 43 3.3.2 Juice and Wine Properties Sterility of pasteurized juice and wine was determined by ATP bioluminescence (Firefly®2 Luminometer, Arrow Scientific). The pH and titratable acidity of juice and wine samples were also measured. Titratable acidity was determined by titration with 0.1N NaOH to an end point of pH 8.1 and calculated as grams of citric acid/L (pH Meter, ColeParmer). Soluble solid content of purees and juices were determined by refractometry (RFM 81 Multi Scale Automatic Refractometer, Bellingham Stanley, Inc.). Ethanol content of wines was determined by ebulliometry (Zoecklein 1990; Dujardin-Salleron Laboratoires). 3.3.3 Culture Preparation Cultures of Escherichia coli O157:H7 (ATCC 43894), Salmonella Typhimurium (ATCC 14028), Listeria monocytogenes (Scott A), and Staphylococcus aureus (general food isolate, 648 From OSU Culture Collection) were used for juice and wine survival studies. All cultures used were from the culture collection at Oregon State University, Department of Food Science and Technology. Cultures were maintained in Trypticase Soy Broth (TSB) then were transferred to fresh TSB and incubated for 24 h at 35°C (BBL™ Trypticase Soy Broth™, BD). One hundred µl from each were then again transferred to fresh TSB and incubated for 18 h at the same temperature. These cultures were then serially diluted in sterile Butterfield’s phosphate buffer (referred to as phosphate buffer for simplicity) and used for inoculation. Enumeration was determined by serial dilution on Trypticase Soy Agar (TSA) (Bacto™ Agar, BD; BBL™ Trypticase Soy Broth™, BD). 44 3.3.4 Survival Study Procedure 3.3.4.1 Controls Due to the presence of pectin, juices were centrifuged at 1613 x g for 5 m prior to use (IEC Clinical Centrifuge). Of each juice supernatant and wine, 9.9 ml was placed in culture tubes, to which 100 µl of a single bacterial strain was added. Samples were serially diluted in phosphate buffer and plated on TSA at appropriate time intervals to determine the maximum survival time of each bacterium in the control samples. 3.3.4.2 Variables Juice supernatant samples were adjusted to have an ethanol content that matched their wine counterpart. For ‘Marion’ juice, 9.405 ml of juice was mixed with 0.495 ml of 100 % ethanol for a total sample volume of 9.9 ml with an ethanol content of 5%. Of ‘Black Diamond’ juice, 9.484 ml was mixed with 0.416 ml of 100% ethanol for a total volume of 9.9 ml with an ethanol content of 4.2%. Wine samples were adjusted with 6M NaOH to increase their pH values by approximately 1 unit in order to evaluate the impact of pH on bacterial survival. One hundred µl of culture was added to each of the variable samples and plated in the method described above for control samples. 3.3.5 Data Analysis All data analyses were conducted using Microsoft Excel. 3.4 Results and Discussion 3.4.1 Properties of Purees, Juices, and Wines The pH of ‘Marion’ and ‘Black Diamond’ purees, juices, and wines were fairly similar, ranging from 3.21 to 3.30 for all products (Tables 3.2-4). The soluble solids 45 content of ‘Marion’ puree and juice was slightly higher than ‘Black Diamond’ puree and juice (Tables 3.2-3). As would be expected based on soluble solids content, ‘Marion’ wine had slightly higher ethanol content than ‘Black Diamond’ wine, at 5.0% and 4.2%, respectively (Table 3.4). Titratable acidity was higher in the ‘Black Diamond’ juice and wine than in the ‘Marion’ juice and wine (Tables 3.3-4). These values are consistent with other reported pH, titratable acidity, and soluble solid content values for blackberry juice (Vasquez-Araujo and Others 2010). Table 3.2 pH and Soluble Solid Content of Blackberry Puree ‘Marion’ Juice ‘Black Diamond’ Juice pH 3.30 3.21 °Brix 12.78 10.88 Table 3.3 pH, Soluble Solid Content, and Titratable Acidity of Blackberry Juices ‘Marion’ Juice ‘Black Diamond’ Juice pH 3.26 3.24 °Brix 11.73 10.85 TA 13.95 g citric acid/L 14.76 g citric acid/L Table 3.4 pH, Ethanol Content, and Titratable Acidity of Blackberry Wines ‘Marion’ Wine ‘Black Diamond’ Wine pH 3.26 3.26 % Ethanol 5% 4.2% TA 15.85 g citric acid/L 15.99 g citric acid/L 3.4.2 Survival Study Results Growth was not observed for any of the microorganisms in any of the treatments. Escherichia coli O157:H7 was observed to no longer be detectable at 84 h in both ‘Marion’ and ‘Black Diamond’ juices (Figures 3.1 and 3.3). The detection limit for 46 the plating procedure used was 0.70 Log CFU/ml. Salmonella Typhimurium was no longer detectable at a maximum of 60 h in ‘Marion’ juice and 108 h in ‘Black Diamond’ juice (Figures 3.5 and 3.7). It should be noted that in ‘Black Diamond’ trials, Salmonella Typhimurium was observed to no longer be detectable at 60 h in one trial, then remained at or near the detection limit from 60-108 h in the second trial (Figure 3.7). This may have been the result of a few particularly acid tolerant cells being present. Staphylococcus aureus survived for 48 and 84 h in ‘Marion’ and ‘Black Diamond’ juices, respectively (Figures 3.9 and 3.11). Results for L. monocytogenes tended to be inconsistent among trials, making it difficult to establish means and ranges. For this reason, results for L. monocytogenes are reported as maximum survival times in Table 3.5 for all treatments. Listeria monocytogenes was observed to have the shortest survival time, at 12 h in both juices (Table 3.5). Adding ethanol to juice samples had the effect of reducing the survival time of all microorganisms, often by more than half. The survival time of E. coli O157:H7 was reduced to 36 h and Salmonella Typhimurium was reduced to 6 h in both juices with added ethanol (Figures 3.1, 3.3, 3.5, and 3.7). The survival time of S. aureus was reduced to 24 h and 36 h, L. monocytogenes to 2 h and 1 h in ‘Marion’ and ‘Black Diamond’ juices with added ethanol, respectively (Figures 3.9 and 3.11, table 3.5). This reduction in survival time was to be expected due to the ability of ethanol to solubilize 47 the bacterial membrane, making it easier for undissociated organic acids to be able to penetrate the bacterial cell (Willey and Others 2006). Escherichia coli O157:H7 was observed to survive for a maximum of 60 m in ‘Marion’ wine and 40 m in ‘Black Diamond’ wine (Figures 3.2 and 3.4). Salmonella Typhimurium and S. aureus were observed to survive for a maximum of 40 m and 80 m in both wine samples, respectively (Figures 3.6, 3.8, 3.10, and 3.12). Listeria monocytogenes survived for a maximum of 80 m in ‘Marion’ wine and 40 m in ‘Black Diamond’ wine (Table 3.5). There was a dramatic difference in survival times when comparing the wine to the juice with added ethanol results, even though both sets of samples had the same ethanol contents and similar pH values. This may have been due to the juice samples still having plenty of nutrients, such as carbohydrates and amino acids, available to the bacterial cells as they attempted to survive the hostile environment of organic acids and ethanol. The wines would have had many of these nutrients depleted by the yeast during the fermentation process. Other differences may include the wine containing additional yeast metabolites that may exhibit antimicrobial activity, such as acetate (Davison and Stephanopoulos 1986). Increasing the pH of the wines had the effect of increasing the survival times of all microorganisms from ≤ 80 m to 6-48 h. In the case of L. monocytogenes, total kill was not observed; however, a 4.62 log reduction occurred in pH adjusted ‘Marion’ wine and 48 a 2.96 log reduction occurred in pH adjusted ‘Black Diamond’ wine at 48 h (Table 3.5). In pH adjusted ‘Marion’ wine, E. coli O157:H7 survived for 36 h, Salmonella Typhimurium for 6 h, and S. aureus for 36 h (Figures 3.1, 3.5, and 3.9). In pH adjusted ‘Black Diamond’ wine, E. coli O157:H7 survived for 48 h, Salmonella Typhimurium for 36 h, and S. aureus for 48 h (Figures 3.3, 3.7, and 3.11). Increasing the pH of the wines had a dramatic effect on the survival time of all microorganisms. This was likely due to the increased pH causing more of the organic acids to exist in their dissociated state, making entry into the bacterial cell more difficult. The dramatic increase in survival observed with L. monocytogenes is consistent with another study that found some strains were able to persist over pH 3.5 and 4.0 for several hours (Phan-Thanh and Others 2000). Figure 3.1 Survival of E. coli O157:H7 in ‘Marion’ Products. Bars indicate the range (high and low values). 7 Log CFU/ml 6 5 Marion Juice 4 Marion Juice Trial 2 Marion Juice 5% ethanol 3 Marion Wine 2 Marion Wine pH 4.31 1 Detection Limit 0 0 20 40 60 Time in Hours 80 49 Figure 3.2 Survival of E. coli O157:H7 in ‘Marion’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 4 Marion Wine 3 Marion WineTrial 2 2 Detection Limit 1 0 0 20 40 60 Time in Minutes Figure 3.3 Survival of E. coli O157:H7 in ‘Black Diamond’ Products. Bars indicate the range (high and low values). 7 6 Black Diamond Juice Log CFU/ml 5 4 Black Diamond Juice 4.2% ethanol 3 Black Diamond Wine 2 Black Diamond Wine pH 4.14 1 Detection Limit 0 0 20 40 Time in Hours 60 80 50 Figure 3.4 Survival of E. coli O157:H7 in ‘Black Diamond’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 Black Diamond Wine 4 3 Black Diamond Wine Trial 1 2 Detection Limit 1 0 0 10 20 30 40 Time in Minutes Figure 3.5 Survival of Salmonella Typhimurium in ‘Marion’ Products. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 Marion Juice 4 Marion Juice Trial 1 3 Marion Juice 5% ethanol Marion Wine 2 Marion Wine pH 4.31 1 Detection Limit 0 0 20 40 Time in Hours 60 51 Figure 3.6 Survival of Salmonella Typhimurium in ‘Marion’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 4 Marion Wine 3 Detection Limit 2 1 0 0 10 20 30 40 50 Time in Minutes Figure 3.7 Survival of Salmonella Typhimurium in ‘Black Diamond’ Products. Bars indicate the range (high and low values). Log CFU/ml 7 6 Black Diamond Juice 5 Black Diamond Juice Trial 1 4 Juice 4.2% Ethanol 3 Black Diamond Wine 2 Wine pH 4.14 1 0 Detection Limit 0 20 40 60 Time in Hours 80 100 52 Figure 3.8 Survival of Salmonella Typhimurium in ‘Black Diamond’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 4 Black Diamond Wine 3 Detection Limit 2 1 0 0 10 20 30 40 50 Time in Minutes Table 3.5 Maximum Observed Survival Times of L. monocytogenes in ‘Marion’ and ‘Black Diamond’ Juices and Wines: All Treatments Treatment ‘Marion’ Juice ‘Marion’ Juice 5.0% Ethanol ‘Marion’ Wine ‘Marion’ Wine pH 4.31 ‘Black Diamond’ Juice ‘Black Diamond’ Juice 4.2% Ethanol ‘Black Diamond’ Wine ‘Black Diamond’ Wine pH 4.14 (Total kill was not observed in pH adjusted wine samples) Survival Time 12 h 2h 80 m 4.62 Log Reduction in 48 h 12h 1h 40 m 2.96 Log Reduction in 48 h 53 Figure 3.9 Survival of S. aureus in ‘Marion’ Products. Bars indicate the range (high and low values). Log CFU/ml 7 6 Marion Juice 5 Marion Juice Trial 1 4 Marion Juice 5.0% Ethanol 3 Marion Wine 2 Marion Wine pH 4.31 1 0 Detection Limit 0 10 20 30 40 50 60 Time in Hours Figure 3.10 Survival of S. aureus in ‘Marion’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 4 Marion Wine 3 Marion Wine Trial 1 Detection Limit 2 1 0 -10 10 30 50 Time in Minutes 70 90 54 Figure 3.11 Survival of S. aureus in ‘Black Diamond’ Products. Bars indicate the range (high and low values). Log CFU/ml 7 6 Black Diamond Juice 5 Black Diamond Juice Trial 1 4 Black Diamond Juice 4.2% Ethanol 3 Black Diamond Wine 2 Black Diamond Wine pH 4.13 1 0 Detection Limit 0 20 40 60 80 Time in Hours Figure 3.12 Survival of S. aureus in ‘Black Diamond’ Wine. Bars indicate the range (high and low values). 7 6 Log CFU/ml 5 4 Black Diamond Wine 3 Black Diamond Trial 1 Detection Limit 2 1 0 0 20 40 60 Time in Minutes 80 55 3.5 Conclusions ‘Marion’ and ‘Black Diamond’ juices and wines did not support the growth of E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus. However, survival will vary depending on acid and ethanol content. The maximum time that any of the tested microorganisms was observed to survive was 80 m in the wines and 108 h in the juices. These findings are consistent with other survival studies conducted using juice and wine made from wine grapes (Just and Daeschel 2003; Sugita-Konishi and Others 2001). These results indicate that if blackberry juice or wine became contaminated post-processing, these particular microorganisms would not be likely to survive by the time the product reached the consumer. Caution should be taken when interpreting these findings for juices because these experiments were conducted at ambient temperatures. If juices were contaminated and held under refrigeration or freezing conditions, survival may be extended. This could be of major concern for products such as unpasteurized frozen puree. Further research would need to be conducted to determine survival times under those conditions. The constituents of the juices and wines that likely contribute to antibacterial activity include organic acids, phenolic compounds, and ethanol (wine). These constituents being present in the same system make it very likely that they act synergistically. The dramatic increase in survival time that was observed when the pH of wines was increased by approximately 1 pH unit indicates that the organic acids are a major antibacterial contributor. Understanding the contribution of each constituent 56 would require conducting survival studies with them individually. Further research would be necessary to fully understand how the phenolic compounds, in the quantities that they occur in blackberry juice and wine, affect the ability of the studied bacteria to survive. 57 4. Overall Conclusions and Future Work The bacterial pathogens used in these studies were not observed to grow on fresh and frozen blackberries. Survival was observed for Listeria monocytogenes and Staphylococcus aureus on fresh, wild ‘Himalaya’ after 3 d and on frozen ‘Triple Crown after 6 months. Salmonella Typhimurium was detected on frozen ‘Triple Crown’ at 3 and 6 months. These results emphasize the need for sanitary growing, harvesting, and handling procedures to prevent contamination. Maintaining such procedures will help ensure that blackberries do not become the center of a food safety incident as raspberries have in the past (Gillesberg and Lassen 2013; Ho and Others 2002; Reid and Robinson 1987; Sarvikivi and Others 2012). Many of the causative agents involved with raspberry recalls are harbored by humans, for example, hepatitis A, norovirus, and Cyclospora cayetanensis. This indicates that blackberries may be susceptible to contamination with microorganisms that humans are known reservoirs for including S. aureus, pathogenic strains of Escherichia coli, and Salmonella spp. in addition to those previously mentioned. Preventing contamination with these microorganisms requires emphasis and attention paid to worker hygiene. Furthermore, considering current recalls, processors are advised to have procedures in place to verify the safety of imported supplies especially if adding them to berry blends. This could be in the form of a certificate of acceptance/analysis or letter of guarantee from a foreign supplier of berry product. 58 Aside from humans, other sources of contamination are possible in the field. Animals, insects, and contaminated soil or irrigation water could all lead to bacterial deposits on blackberry fruit (Beuchat 2002; Janisiewicz and Others 1999; Terry 2011). The mechanical harvester evaluated did not appear to a potential source of contamination, even when left intentionally unwashed. A diverse microflora was observed on the surface of fresh blackberries. How this microflora affects the ability of pathogenic bacteria to adhere to the berry surface and survive is not well understood and may be worth investigating further. The inability of E. coli O157:H7, Salmonella Typhimurium, L. monocytogenes, and S. aureus to survive beyond 80 m in wines and 108 h in juices demonstrate that blackberries inherently have antibacterial properties. There are several constituents of blackberry juices and wines that are likely to contribute to bacterial death, including organic acids, phenolic compounds, and ethanol in the case of wines. These constituents likely behave synergistically to cause bacterial cells to die. The dramatic increase in survival time observed when the pH of the wines was increased suggests that the organic acids are the primary antibacterial constituent. These studies were conducted at ambient temperatures. Future work should look at what effect the sample temperature has on survival and should be extended to frozen blackberry puree. Furthermore, conducting survival studies with isolated phenolic compounds from blackberries may yield valuable information. 59 Bibliography Aura A, Martin-Lopez P, O’Leary KA & Others. (2005). In Vitro Metabolism of Anthocyanins by Human Gut Flora. European Journal of Nutrition 44: 133-42. Beuchat LR. (1987). Food and Beverage Mycology. 2nd ed. New York: Van Nostrand Reinhold. 101 p. Beuchat LR. (2002). Ecological Factors Influencing Survival and Growth of Human Pathogens on Raw Fruits and Vegetables. Microbes and Infection 4: 413-23. Brul S & Coote P. (1999). Preservative Agents in Foods: Mode of Action and Microbial Resistance Mechanisms. International Journal of Food Microbiology 50:1-17. Bilyk A & Sapers GM. (1986). Varietal Differences in the Quercetin, Kaempferol, and Myricetin Contents of Highbush Blueberry, Cranberry, and Thornless Blackberry Fruits. Journal of Agricultural and Food Chemistry 34(4): 585-8. Bowling B. (2000). The Berry Grower’s Companion. Portland: Timbers Press. 93-132 p. [CDC] Centers for Disease Control and Prevention. (2010). State-Specific Trends in Fruit and Vegetable Consumption Among Adults-United States, 2000-2009. Morbidity and Mortality Weekly Report 59(35):1125-1130. [CDC] Centers for Disease Control and Prevention. (2011). Strategies to Prevent Obesity and Other Chronic Diseases: The CDC Guide to Strategies to Increase the Consumption of Fruits and Vegetables. Atlanta: U.S. Department of Health and Human Services [CDC] Centers for Disease Control and Prevention. (2013). Multistate Outbreak of Hepatitis A infections Linked to Pomegranate Seeds from Turkey. [Accessed June 28, 2013] http://www.cdc.gov/hepatitis/Outbreaks/2013/A1b-03-31/ Davison BH & Stephanopoulos G. (1986). Coexistence of S. cerevisiae and E. coli in Hemostat Under Substrate Competition and Product Inhibition. Biotechnology & Bioengineering 28(11):1742-52. Du XF, Kurnianta A, McDaniel M, & Others. (2010). Flavour Profiling of ‘Marion’ and Thornless Blackberries by Instrumental and Sensory Analysis. Food Chemistry 121:10808. 60 Duan J and Zhao Y. (2009). Antimicrobial Efficiency of Essential Oil and Freeze-Thaw Treatments against Escherichia coli O157:H7 and Salmonella enterica Ser. Enteritidis in Strawberry Juice. Journal of Food Science 74(3):M131-7. Falkenhorst G, Krusell L, Lisby M & Others. (2005). Imported Frozen Raspberries Cause a Series of Norovirus Outbreaks in Denmark, 2005. Eurosurveillance 10(38): pii=2795. [Accessed June 27, 2013] Available online: http://www.eurosurveillance.org/ViewArticle.aspx?ArticleId=2795 Fan-Chian, H. December 14, 1999. Anthocyanin Pigment, Nonvolatile Acid and Sugar Composition of Blackberries, MS Thesis. Corvallis, OR: Oregon State University. 90p. [Accessed June 29, 2013] Available from Oregon State University Scholars Archive: http://ir.library.oregonstate.edu/xmlui/bitstream/handle/1957/13758/FanChiangHoju1 999.pdf?sequence=1 Finn CE, Yorgey BM, Strik BC & Others. (2005). ‘Metilius’ Trailing Blackberry. HortScience 40(7):2189-91. Finn CE and Strik BC. (2008). Blackberry Cultivars for Oregon. Oregon State University Extension Service. EC 1617-E. Flegal KM, Carroll MD, Kit BK, & Others. (2012). Prevalence of Obesity and Trends in the Distribution of Body Mass Index Among US Adults, 1999-2010. Journal of the American Medical Association 307(5):491-7. [FDA] Food and Drug Administration. (2011). Fresh Strawberries from Washington County Farm Implicated in E. coli O157 Outbreak in NW Oregon. [Accessed June 28, 2013] http://www.fda.gov/safety/recalls/ucm267667.htm Friedman M, Henika PR, Levin CE & Others. (2004). Antibacterial Activities of Plant Essential Oils and Their Components against Escherichia coli O157:H7 and Salmonella enterica in Apple Juice. Journal of Agricultural and Food Chemistry 52:6042-8. Gillesberg Lassen S, Soborg B, Midgley SE & Others. (2013). Ongoing Multi-strain Foodborne Hepatitis A Outbreak with Frozen Berries as Suspected Vehicle: Four Nordic Countries Affected, October 2012 to April 2013. Eurosurveillance 18(17):pii= 20467. Gropper SS, Smith JL, and Groff JL. (2008) Advanced Nutrition and Human Metabolism. 5th ed. Belmont: Wadsworth. 55, 113, 264 p. 61 Herwaldt BL, Ackers ML and the Cyclospora Working Group. (1997). An Outbreak in 1996 of Cyclosporiasis Associated with Imported Raspberries. New England Journal of Medicine 336(22):1548-56. Ho AY, Lopez AS, Eberhart MG & Others. (2002). Outbreak of Cyclosporiasis Associated with Imported Raspberries, Philadelphia, Pennsylvania, 2000. Emerging Infectious Diseases 8(8):783-8. Hummer K. (2010). Rubus Pharmacology: Antiquity to the Present. HortScience 45(11): 1587-91. Janisiewicz W, Conway WS, Brown MW & Others. (1999). Fate of Escherichia coli O157:H7 on Fresh-But Apple Tissue and Its Potential for Transmission by Fruit Flies. Applied Environmental Microbiology 65(1): 1-5. Jay JM, Loessner MJ, & Golden DA. (2005). Modern Food Microbiology. 7th ed. New York: Springer Science. 39-59, 401 p. Jenkins DJA, Kendall CWC, Vuksan V & Others. (2002). Soluble Fiber Intake at a Dose Approved by the US Food and Drug Administration for a Claim of Health Benefits: Serum Lipid Risk Factors for Cardiovascular Disease Assessed in a Randomized Controlled Crossover Trial. The American Journal of Clinical Nutrition 75:834-9. Jensen B, Knudsen IMB, Andersen B & Others. (2013). Characterization of Microbial Communities and Fungal Metabolites on Field Grown Strawberries from Organic and Conventional Production. International Journal of Food Microbiology 160:313-22. Just JR & Daeschel MA. (2003). Antimicrobial Effects of Wine on Escherichia coli O157:H7 and Salmonella Typhimurium in a Model Stomach System. Journal of Food Science 68(1): 285-90. Kempler K & Humpf HU. (2005). Metabolism of Anthocyanins and their Phenolic Degradation Products by the Intestinal Microflora. Bioorganic and Medicinal Chemistry 13: 5195-205. Knudsen DM, Yamamoto SA, & Harris LJ. (2001). Survival of Salmonella spp. And Escherichia coli O157:H7 on Fresh and Frozen Strawberries. Journal of Food Protection 64(10):1483-8. 62 Mahmoud BSM, Bachman G, & Linton RH. (2010). Inactivation of Escherichia coli O157:H7, Listeria monocytogenes, Salmonella enterica and Shigella flexneri on Spinach Leaves by X-ray. Food Microbiology 27:24-8. Nohynek LJ, Alakomi H, Kahkonen MP & Others. (2006). Berry Phenolics: Antimicrobial Properties and Mechanisms of Action Against Severe Human Pathogens. Nutrition and Cancer 54(1):18-32. Oregon Climate Service. (July 2011). College of Oceanic and Atmospheric Sciences: Oregon State University. [Accessed June 21, 2013]. Available online: http://www.ocs.orst.edu/wp-content/uploads/2011/11/juneOCS.pdf Oyarzabal OA, Nogueira MCL & Gombas DE. (2003). Survival of Escherichia coli O157:H7, Listeria monocytogenes, and Salmonella in Juice Concentrates. Journal of Food Protection 66(9):1595-8. Perrigue M, Carter B, Roberts SA, & Others. (2010). A Low-Calorie Beverage Supplemented with Low-Viscosity Pectin Reduces Energy Intake at a Subsequent Meal. Journal of Food Science 275(9): H300-5. Phan-Thanh L, Mahouin F & Alige S. (2000). Acid Responses of Listeria monocytogenes. International Journal of Food Microbiology 55:121-6. Puupponen-Pimia R, Nohynek L, Meier C & Others. (2001). Antimicrobial Properties of Phenolic Compounds from Berries. Journal of Applied Microbiology 90: 494-507. Puupponen-Pimia R, Nohynek L, Alakomi H & Others. (2005). Bioactive Berry Compounds-Novel Tools Against Human Pathogens. Applied Microbiology and Biotechnology 67: 8-18. Raybaudi-Massilia RM, Mosqueda-Melgar J, & Martin-Belloso O. (2006). Antimicrobial Activity of Essential Oils on Salmonella enteritidis, Escherichia coli, and Listeria innocua in Fruit Juices. Journal of Food Protection 69(7): 1579-1586. Reid TMS & Robinson HG. (1987). Frozen Raspberries and Hepatitis A. Epidemiological Infection 98:109-12. Rico D, Martin-Diana AB, Barat JM & Others. (2007). Extending and Measuring the Quality of Fresh-cut Fruit and Vegetables: A Review. Trends in Food Science & Technology 18:373-86. 63 Ruyi W, Frei B, Kennedy JA & Others. (2010). Effects of Refrigerated Storage and Processing Technologies on the Bioactive Compounds and Antioxidant Capacities of ‘Marion’ and ‘Evergreen’ Blackberries. Food Science and Technology 43: 1253-64. Sarvikivi E, Roivainen M, Maunula L & Others. (2012). Multiple Norovirus Outbreaks Linked to Imported Frozen Raspberries. Epidemiology and Infection 140:260-7. Sasaki R, Nishimura N, Hoshino H, & Others. (2007). Cyanidin-3-glucoside Ameliorates Hyperglycemia and Insulin Sensitivity Due to Downregulation of Retinol Binding Protein 4 Expression in Diabetic Mice. Biochemical Pharmacology 74: 1619-27. Sellappan S, Akoh CC & Krewer G. (2002). Phenolic Compounds and Antioxidant Capacity of Georgia-Grown Blueberries and Blackberries. Journal of Agricultural and Food Chemistry 50: 2432-8. Shepherd T & Griffiths DW. (2006).The Effects of Stress on Plant Cuticular Waxes. New Phytologist 171:469-99. Stone C. (2011). Fresh Strawberries Implicated in E. coli O157 Outbreak in NW Oregon. New York Berry News 10(7):1. Strik BC, Clark JR, Finn CE & Others. (2007). Worldwide Blackberry Production. HortTechnology 17(2): 205-13. Sugita-Konishi Y, Hara-Kudo Y, Iwamoto T & Others. (2001). Wine has Activity against Entero-pathogenic Bacteria in Vitro but not in Vivo. Bioscience, Biotechnology, and Biochemistry 65(4):954-7. Tournas VH & Katsoudas E. (2005). Mould and Yeast Flora in Fresh Berries, Grapes and Citrus Fruits. International Journal of Food Microbiology 105:11-17. Terry L. (2013). Hepatitis A Outbreak: Gresham Company Recalls Pomegranate Seeds. The Oregonian, June 27, 2013. [Accessed June 28, 2013] http://www.oregonlive.com/health/index.ssf/2013/06/hepatitis_a_outbreak_gresham_ c.html Terry L. (2011). Tests Reveal E. coli in Deer Droppings Found in Oregon Strawberry Field. The Oregonian. August 11, 2011. [Accessed April 25, 2013] http://www.oregonlive.com/washingtoncounty/index.ssf/2011/08/tests_reveal_e_coli_ in_deer_dr.html 64 Tschriter O, Fritsche A, Thamer C & Others. (2003). Plasma Adiponectin Concentrations Predict Insulin Sensitivity of Both Glucose and Lipid Metabolism. Diabetes 52: 239-43. Tsuda, T. (2012). Dietary Anthocyanin-rich Plants: Biochemical Basis and Recent Progress in Health Benefits Studies. Molecular Nutrition and Food Research 56:159-70. [USDA]. United States Department of Agriculture. National Nutrient Database for Standard Reference. Blackberries, Raw.[Accessed May 5, 2013] http://ndb.nal.usda.gov/ndb/foods/show/2180 [USDA] United States Department of Agriculture. (2012). Noncitrus Fruits and Nuts 2011 Preliminary Summary. Vasquez-Araujo, L, Chambers IV E, Adhikari K & Others. (2010). Sensory and Physicochemical Characterization of Juices Made with Pomegranate and Blueberries, Blackberries, or Raspberries. Journal of Food Science 75(7):S398-404. Willey JM, Sherwood LM, & Woolverton CJ. (2008). Prescott, Harley, & Klein’s Microbiology. Customized Version for Oregon State University, 7th ed. Indianapolis: McGraw Hill Learning Solutions. 159-60 p. Yao LH, Jiang YM, Shi J & Others. (2004). Flavonoids in Foods and Their Health Benefits. Plant Foods for Human Nutrition 59: 113-22. Zoecklein BW, Fugelsang KC, Gump BH & Others. (1990). Production Wine Analysis. New York: Van Nostrand Reinhold International Company. 3-34, 43-5, 157-6 p. 65 APPENDICES 66 Appendix I. Fresh Field Samples Raw Data, Chapter 2. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/g or 0.70 Log CFU/g. Table I.1 Aerobic Plate Count Raw Data, Fresh Samples Rep 1 Dilution on Plate 10^-3 10^-4 10^-5 10^-6 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 1 0 0 1 17 0 0 0 9000 3.95 15 5 0 0 31 5 0 0 23000 4.36 Plate 2 CFU/ g Log CFU/g 65 70 15 12 0 0 0 Contaminated 6750 3.83 Rep 1 Dilution on Plate 10^-2 10^-3 10^-4 10^-5 10^-2 10^-3 10^-4 10^-5 Obsidian' Late-Harvest 07/29/11 Rep 2 Plate 1 Plate 2 CFU/g Log CFU/g 221 46 27 1 228 34 0 2 31225 4.49 Rep 1 Dilution on Plate 'Obsidian' Mid Harvest 07/20/11 Rep 2 Plate 1 'Triple Crown' Early-Harvest 08/23/11 Rep 2 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 38 2 1 0 28 7 0 0 3300 3.52 42 6 1 2 37 8 0 0 3950 3.60 Triple Crown' Mid/Late Harvest 08/30/11 Rep 1 Rep 2 Dilution on Plate 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g TNTC 56 13 2 TNTC 27 7 3 41500 4.62 243 20 2 0 206 14 1 0 22450 4.35 67 Table I.2 Yeasts and Molds Raw Data, Fresh Samples 'Obsidian' Mid-Harvest 07/20/11 Rep 2 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g TNTC 107 13 TNTC 29 5 6800 3.83 TNTC 300 29 TNTC 550 40 34500 4.53 Obsidian' Late-Harvest 07/29/11 Rep 2 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g TNTC 257 63 TNTC 231 74 53367 4.73 TNTC 239 50 TNTC 270 49 40967 4.61 'Triple Crown' Early-Harvest 08/23/11 Rep 2 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 141 16 1 97 24 2 1190 3.01 117 29 1 100 33 10 2093 3.32 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Triple Crown' Mid/Late Harvest 08/30/11 Rep 2 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 209 68 15 170 77 14 4572 3.66 185 102 3 210 85 9 5663 3.75 68 Table I.3 Coliforms Raw Data, Fresh Samples 'Obsidian' Mid-Harvest 07/20/11 Rep 2 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 0 0 0 0 0 0 <5 <0.70 11 0 0 14 0 0 125 2.10 'Obsidian' Late-Harvest 07/29/11 Rep 2 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 0 0 0 0 0 0 <5 <0.70 0 0 0 0 0 0 <5 <0.70 Rep 1 'Triple Crown' Early-Harvest 08/23/11 Rep 2 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 4 0 0 1 0 0 25 1.40 0 0 0 0 0 0 <5 <0.70 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 'Triple Crown' Mid/Late-Harvest 08/30/11 Rep 2 Plate 1 Plate 2 CFU/g Log CFU/g Plate 1 Plate 2 CFU/g Log CFU/g 0 0 0 0 0 0 <5 <0.70 0 0 0 0 0 0 <5 <0.70 69 Appendix II. Mechanical Harvester Raw Data and Photos, Chapter 2. Bold indicates value used in calculation. Table II.1 Aerobic Plate Count Raw Data, Harvester Location 1 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 CFU/swab Log CFU/swab 2.95 TNTC TNTC 4600 53 39 4 0 Location 2 Pre-Harvest Post-Harvest 3.66 TNTC TNTC 6 12 2 1 Plate 1 Plate 2 216 2 10 227 31 11 Plate 1 Plate 2 CFU/swab Post-Harvest Log CFU/swab Plate 1 900 CFU/swab 2510 Log CFU/swab Plate 1 Plate 2 CFU/swab 3.40 TNTC 38 5 Location 3 350 34 3 3600 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 TNTC TNTC 11 TNTC 37 63 Plate 2 CFU/swab 50000 Log CFU/swab 3.56 Post-Harvest Log CFU/swab Plate 1 Plate 2 CFU/swab 4.70 41 2 0 52 4 1 Log CFU/swab Plate 1 Plate 2 CFU/swab Log CFU/swab 2.29 221 24 1 171 22 0 1960 3.29 465 Log CFU/swab 2.67 Location 4 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 14 1 0 25 2 0 CFU/swab 195 Post-Harvest Location 5 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 350 TNTC 43 41 21 3 CFU/swab 4200 Post-Harvest Log CFU/swab Plate 1 Plate 2 3.62 400 47 2 350 44 20 CFU/swab 4500 Log CFU/swab 3.66 Location 6 Pre-Harvest Dilution on Plate Plate 1 Plate 2 CFU/swab Post-Harvest Log CFU/swab Plate 1 Plate 2 CFU/swab Log CFU/swab 70 10^-1 10^-2 10^-3 88 9 0 101 4 1 945 2.98 221 24 1 171 22 0 1960 3.29 Location 7 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 9 0 0 31 7 0 CFU/swab 200 Post-Harvest Log CFU/swab Plate 1 Plate 2 2.30 27 3 2 23 2 0 Log CFU/swab Plate 1 Plate 2 1 111 12 7 88 13 13 CFU/swab 250 Log CFU/swab 2.40 Location 8 Pre-Harvest Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 0 0 0 2 0 0 CFU/swab Figure II.1 Harvester Location 1 10 Post-Harvest CFU/swab Figure II.2 Harvester Location 2 995 Log CFU/swab 2.99 71 Figure II-3 Harvester Location 3 Figure II.5 Harvester Location 5 Figure II.4 Harvester Location 4 (beater bar) Figure II.6 Harvester Location 6 72 Figure II.7 Harvester Location 7 Figure II.8 Harvester Location 8 Appendix III. ‘Himalaya’ Raw Data, Chapter 2. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/g or 0.70 Log CFU/g; 1/0.02 = 50 CFU/g or 1.70 Log CFU/g for homogenized samples. Table III.1 E. coli O157:H7 on fresh 'Himalaya' Blackberries, Raw Data Rep 1 Berry Weight 1.4 Inoculum 5.74 g Rep 2 1.6 Log CFU/g g 5.69 Log CFU/g Rinse Solution Dilution on Plate 10^-1 10^-2 10^-3 Homogenized 1:10 Dilution on Plate Plate 1 Plate 2 Survivors Log CFU/g Plate 1 Plate 2 Survivors Log CFU/g 0 0 0 0 0 0 <5 <0.70 0 0 0 0 0 0 <5 <0.70 73 10^-2 0 0 10^-3 0 0 <50 <1.70 0 0 0 0 <50 <1.70 Table III.2 Salmonella Typhimurium on fresh 'Himalaya' Blackberries, Raw Data Rep 1 Rep 2 Berry Weight 1.3 Inoculum 5.80 g 1.1 Log CFU/g 5.87 g Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 Survivors Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 Log CFU/g <0.70 0 4 0 0 0 0 0 10^-2 0 0 0 0 <50 <1.70 10^-3 0 0 0 0 <5 Homogenized 1:10 Dilution on Plate <50 <1.70 Table III.3 L. monocytogenes on fresh 'Himalaya' Blackberries, Raw Data Rep 1 Berry Weight 1 Inoculum 6.25 g Rep 2 0.6 Log CFU/g g 6.47 Log CFU/g Plate 1 0 Plate 2 0 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 Survivors 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 0 0 0 0 10^-3 0 0 0 0 <5 Log CFU/g <0.70 <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate <50 <1.70 74 Table III.4 S. aureus on fresh 'Himalaya' Blackberries, Raw Data Rep 1 Berry Weight 1.2 Inoculum 5.33 Rep 2 g 1.7 Log CFU/g g 5.18 Log CFU/g Plate 1 0 Plate 2 0 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 Survivors Log CFU/g <0.70 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 2 2 1 0 10^-3 0 0 0 0 <5 <5 Log CFU/g <0.70 50 1.70 Homogenized 1:10 Dilution on Plate 200 2.30 Appendix IV. ‘Triple Crown’ Raw Data, Chapter 2. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/g or 0.70 Log CFU/g; 1/0.02 = 50 CFU/g or 1.70 Log CFU/g for homogenized samples. Table IV.1 E. coli O157:H7 on Frozen 'Triple Crown' Blackberries, Raw Data Rep 1 Rep 2 Berry Weight 8.7 Inoculum 4.40 g 6.9 Log CFU/g 4.50 g Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 0 10^-2 0 0 10^-3 0 0 Survivors Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 Log CFU/g <0.70 0 0 0 0 0 0 0 0 <50 <1.70 0 0 <5 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 3 Berry Weight Inoculum Rinse Solution Rep 4 7.7 4.45 g Log CFU/g 8.3 4.42 g Log CFU/g 75 Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 0 10^-2 0 0 10^-3 0 0 Survivors Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 Log CFU/g <0.70 0 0 0 0 0 0 0 0 <50 <1.70 0 0 <5 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 5 Berry Weight Rep 6 10 Inoculum g 4.34 9.6 Log CFU/g 4.36 g Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 Survivors Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 Log CFU/g <0.70 0 0 0 0 0 0 0 10^-2 0 0 0 0 <50 <1.70 10^-3 0 0 0 0 <5 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 7 Berry Weight 10.6 g Inoculum 4.31 Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 0 10^-3 0 0 10^-2 0 0 10^-3 0 0 Survivors <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate 76 Table IV.2 Salmonella Typhimurium on Frozen 'Triple Crown' Blackberries, Raw Data Rep 1 at 3 months Rep 2 Berry Weight 9.5 Inoculum 3.95 g 10.5 g Log CFU/g 3.90 Log CFU/g Plate 1 0 Plate 2 0 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 1 Plate 2 1 Survivors Log CFU/g 1.00 10^-2 0 1 0 0 10^-3 0 0 0 0 10^-2 0 0 0 0 10^-3 0 0 0 0 10 <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 3 Berry Weight Rep 4 7.7 Inoculum 4.04 g 9.3 Log CFU/g g 3.96 Log CFU/g Plate 1 0 Plate 2 0 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 Survivors Log CFU/g <0.70 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 0 0 0 0 10^-3 0 0 0 0 <5 <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 5 Rep 6 Berry Weight 10.3 g 11.3 g Inoculum 3.91 Log CFU/g 3.87 Log CFU/g Plate 1 0 Plate 2 0 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 1 Plate 2 0 10^-2 0 0 0 0 10^-3 0 0 0 0 Homogenized 1:10 Dilution on Plate Survivors 5 Log CFU/g 0.70 <5 Log CFU/g <0.70 77 10^-2 0 0 10^-3 0 0 <50 <1.70 0 0 0 1 <50 <1.70 Rep 7 Berry Weight 8.4 Inoculum 4.00 g Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 0 10^-3 0 0 10^-2 0 0 10^-3 0 0 Survivors <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate Table IV.3 L. monocytogenes on Frozen 'Triple Crown' Blackberries, Raw Data Rep 1 Rep 2 Berry Weight 9.6 Inoculum 4.32 g 7.7 Log CFU/g g 4.42 Log CFU/g Plate 1 1 Plate 2 1 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 Survivors Log CFU/g <0.70 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 0 1 2 0 10^-3 0 0 0 0 <5 10 Log CFU/g 1 100 2 Homogenized 1:10 Dilution on Plate 50 1.70 Rep 3 Rep 4 Berry Weight 11.5 g 9.8 Inoculum 4.24 Log CFU/g 4.31 g Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 0 Survivors <5 Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 0 0 Log CFU/g <0.70 78 10^-3 0 0 10^-2 0 0 10^-3 0 0 0 0 0 0 0 0 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 5 Berry Weight <1.70 Rep 6 5.7 Inoculum <50 4.55 g 11.7 g Log CFU/g 4.24 Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 Survivors Log CFU/g <0.70 Plate 1 0 Plate 2 Survivors 0 <5 Log CFU/g <0.70 0 0 0 0 0 0 0 10^-2 0 0 0 1 50 1.70 10^-3 0 0 0 0 <5 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 7 Berry Weight 10.8 g Inoculum 4.27 Log CFU/g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 0 10^-3 0 0 10^-2 0 0 10^-3 0 0 Survivor s <5 Log CFU/g <0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate Table IV.4 S. aureus on Frozen 'Triple Crown' Blackberries, Raw Data Rep 1 Berry Weight Inoculum Rinse Solution 8.7 3.59 g Log CFU/g Rep 2 7.8 3.63 g Log CFU/g 79 Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 10^-3 0 10^-2 2 1 10^-3 0 0 Survivors Log CFU/g <0.70 Plate 1 1 Plate 2 0 0 0 0 0 0 0 0 0 0 0 <5 Survivors 5 Log CFU/g 0.70 <50 <1.70 Homogenized 1:10 Dilution on Plate 150 2.18 Rep 3 Berry Weight Rep 4 8.9 Inoculum 3.58 g 9.3 Log CFU/g g 3.56 Log CFU/g Plate 1 1 Plate 2 1 Survivors Rinse Solution Dilution on Plate 10^-1 Plate 1 1 Plate 2 0 Survivors Log CFU/g 0.70 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 0 0 1 0 10^-3 0 0 0 0 5 10 Log CFU/g 1.00 50 1.70 3.54 Log CFU/g Plate 1 0 Plate 2 0 Survivors <5 Log CFU/g 0.70 100 2.00 Homogenized 1:10 Dilution on Plate <50 <1.70 Rep 5 Berry Weight Rep 6 8.5 Inoculum 3.60 g 9.6 Log CFU/g g Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 Survivors Log CFU/g 0.70 10^-2 0 0 0 0 10^-3 0 0 0 0 10^-2 5 12 2 0 10^-3 0 0 0 0 <5 Homogenized 1:10 Dilution on Plate 850 2.93 Rep 7 Berry Weight Inoculum 7.9 3.63 g Log CFU/g 80 Rinse Solution Dilution on Plate 10^-1 Plate 1 0 Plate 2 0 10^-2 0 0 10^-3 0 0 10^-2 1 0 10^-3 0 0 Survivors <5 Log CFU/g <0.70 50 1.70 Homogenized 1:10 Dilution on Plate Appendix V. Juice Raw Data, Chapter 3. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/ml or 0.70 Log CFU/ml. Table V.1 E. coli O157:H7 in 'Marion' Juice, Raw Data Rep 1 12/14/11 Time Dilution on Plate Plate 1 Plate 2 6h 10^-1 TNTC TNTC 10^-2 TNTC TNTC 10^-3 112 127 10^-4 25 28 10^-5 0 4 10^-6 1 0 12h 10^-1 TNTC TNTC 10^-2 194 215 10^-3 56 46 10^-4 6 8 10^-5 0 0 10^-6 0 0 24h 10^-1 TNTC TNTC 10^-2 66 98 10^-3 10 3 36h 10^-1 91 82 10^-2 0 2 48h 10^-1 0 0 60h 10^-1 --72h 10^-1 --84h 10^-1 --Rep 2 8/22/12 Survivors 192250 Log CFU/ml 5.28 35725 4.55 8200 3.91 865 2.94 <5 <0.70 81 Time 6h 12h 24h 36h 48h 60h 72h 84h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 -10^-1 10^-2 10^-3 10^-4 10^-5 -10^-6 -10^-1 10^-2 10^-3 10^-1 10^-2 10^-1 10^-1 10^-1 10^-1 Plate 1 TNTC TNTC 223 44 7 Plate 2 TNTC TNTC 191 34 2 Survivors 298500 Log CFU/ml 5.474 TNTC TNTC 105 14 108500 5.04 TNTC 78 6 24 0 0 1 0 0 7000 3.85 230 2.36 20 10 5 <5 1.30 1.00 0.70 <0.70 Survivors 84500 Log CFU/ml 4.93 14500 4.16 1570 3.20 -TNTC TNTC 112 19 --TNTC 62 13 22 1 4 1 1 0 Table V.2 E. coli O157:H7 in 'Black Diamond' Juice, Raw Data Rep 1 12/14/11 Time Dilution on Plate Plate 1 Plate 2 6h 10^-1 TNTC TNTC 10^-2 300 300 10^-3 85 84 10^-4 15 15 10^-5 2 1 10^-6 0 0 12h 10^-1 TNTC TNTC 10^-2 156 134 10^-3 23 10 10^-4 5 1 10^-5 2 0 10^-6 0 0 24h 10^-1 125 189 10^-2 18 7 82 36h 48h 60h 72h 84h Time 6h 12h 24h 36h 48h 60h 72h 84h 10^-3 10^-1 10^-2 106-3 10^-1 10^-1 10^-1 10^-1 0 1 0 -- Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 -10^-1 10^-2 10^-3 10^-4 10^-5 -10^-6 -10^-1 10^-2 10^-3 10^-1 10^-2 10^-3 10^-1 10^-1 10^-1 10^-1 1 3 0 20 1.30 5 5 10 <5 0.70 0.70 1.00 <0.70 Survivors 327250 Log CFU/ml 5.51 58000 4.76 4800 3.68 275 2.44 30 15 10 <5 1.48 1.18 1.00 <0.70 -1 1 2 0 0 0 0 0 Rep 2 8/22/12 Plate 1 Plate 2 TNTC TNTC TNTC TNTC 155 194 45 51 3 3 -TNTC TNTC TNTC TNTC 54 62 10 12 --TNTC TNTC 54 42 8 8 28 27 1 1 1 0 5 1 3 0 2 0 0 0 Table V.3 Salmonella Typhimurium in 'Marion' Juice, Raw Data Rep 1 12/14/11 Time Dilution on Plate Plate 1 Plate 2 Survivors 6h 10^-1 TNTC TNTC 11750 10^-2 85 150 10^-3 18 21 10^-4 5 7 Log CFU/ml 4.07 83 12h 24h 36h 48h 60h Time 6h 12h 24h 36h 48h 60h 10^-5 10^-6 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-1 10^-1 10^-1 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-1 10^-1 10^-1 -- ------ -- 0 0 0 0 219 131 13 6 1 0 0 0 0 0 0 0 12 13 2 0 3 2 1 2 0 0 Rep 2 08/14/12 Plate 1 Plate 2 57 58 2 3 1 0 0 0 --21 16 1 1 ----1 2 -1 0 0 0 -- 1750 3.24 125 2.10 25 15 <5 1.40 1.18 <0.70 Survivors 575 Log CFU/ml 2.76 185 2.27 15 1.18 5 <5 0.70 <0.70 Table V.4 Salmonella Typhimurium in 'Black Diamond' Juice, Raw Data Rep 1 12/14/11 Time Dilution on Plate Plate 1 Plate 2 Survivors 6h 10^-1 TNTC TNTC 7325 10^-2 142 151 10^-3 24 21 10^-4 4 2 Log CFU/ml 3.86 84 12h 24h 36h 48h 60h 72h 84h 96h 108h Time 6h 12h 24h 36h 48h 60h 72h 84h 96h 108h 10^-5 10^-6 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-1 10^-1 10^-1 10^-1 10^-1 10^-1 10^-1 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 10^-1 10^-2 10^-1 10^-1 10^-1 10^-1 10^-1 10^-1 10^-1 --- ------ ----- 0 0 0 0 37 34 1 3 1 1 0 0 0 0 0 0 3 7 0 0 4 2 1 6 0 1 1 2 1 1 1 0 0 0 Rep 2 08/14/12 Plate 1 Plate 2 76 67 3 2 0 0 0 0 --26 31 0 0 ----36 3 -3 1 2 1 0 0 ----- 355 2.55 50 1.70 30 35 5 15 10 5 <5 1.48 1.54 0.70 1.18 1.00 0.70 <0.70 Survivors 715 Log CFU/ml 2.85 285 2.45 195 2.29 20 15 <5 1.30 1.18 <0.70 85 Table V.5 L. monocytogenes in 'Marion' Juice, Raw Data Rep 1 03/03/12 Time Dilution on Plate Plate 1 Plate 2 3h 10^-1 --10^-2 --10^-3 --10^-4 --6h 10^-1 35 51 10^-2 1 0 10^-3 0 0 10^-4 0 0 10^-5 0 0 10^-6 0 0 12h 10^-1 0 0 10^-2 0 0 10^-3 0 0 10^-4 0 0 10^-5 0 0 Rep 2 09/05/12 Time Dilution on Plate Plate 1 Plate 2 3h 10^-1 2 5 10^-2 0 0 10^-3 0 0 10^-4 0 0 6h 10^-1 0 0 10^-2 0 0 10^-3 --10^-4 --10^-5 --10^-6 --12h 10^-1 --10^-2 --10^-3 --10^-4 --10^-5 --- Survivors Log CFU/ml 430 2.63 <5 <0.70 Survivors 35 Log CFU/ml 1.54 <5 <0.70 86 Table V.6 L. monocytogenes in 'Black Diamond' Juice, Raw Data Rep 1 03/03/12 Time Dilution on Plate Plate 1 Plate 2 Survivors 3h 10^-1 --10^-2 --10^-3 --10^-4 --6h 10^-1 10 16 130 10^-2 0 0 10^-3 0 0 10^-4 0 0 10^-5 0 0 10^-6 0 0 12h 10^-1 0 0 <5 10^-2 0 0 10^-3 0 0 10^-4 0 0 10^-5 0 0 Rep 2 09/05/12 Time Dilution on Plate Plate 1 Plate 2 Survivors 3h 10^-1 0 0 <5 10^-2 0 0 10^-3 0 0 10^-4 0 0 6h 10^-1 0 0 10^-2 --10^-3 --10^-4 --10^-5 --10^-6 --12h 10^-1 --10^-2 --10^-3 --10^-4 --10^-5 --- Log CFU/ml 2.11 <0.70 Log CFU/ml <0.70 87 Table V.7 S. aureus in 'Marion' Juice, Raw Data Rep 1 04/11/12 Time Dilution on Plate Plate 1 Plate 2 6h 10^-1 TNTC TNTC 10^-2 290 230 10^-3 30 27 10^-4 --12h 10^-1 TNTC TNTC 10^-2 109 139 10^-3 --10^-4 --24h 10^-1 208 206 10^-2 19 10 36h 10^-1 2 2 10^-2 0 0 48h 10^-1 0 0 Rep 2 09/18/12 Time Dilution on Plate Plate 1 Plate 2 6h 10^-1 80 101 10^-2 5 5 10^-3 0 0 10^-4 0 0 12h 10^-1 2 3 10^-2 0 0 10^-3 0 0 10^-4 0 0 24h 10^-1 0 0 10^-2 0 0 36h 10^-1 --10^-2 --48h 10^-1 --- Table V.8 S. aureus in 'Black Diamond' Juice, Raw Data Rep 1 03/23/12 Time Dilution on Plate Plate 1 Plate 2 6h 10^-1 TNTC TNTC 10^-2 126 71 10^-3 8 15 10^-4 12h 10^-1 TNTC TNTC Survivors 26667 Log CFU/ml 4.43 12400 4.09 2070 3.32 20 1.30 <5 <0.70 Survivors 905 Log CFU/ml 2.96 25 1.40 <5 <0.70 Survivors 9850 Log CFU/ml 3.99 8100 3.91 88 24h 36h 48h 60h 72h 84h Time 6h 12h 24h 36h 48h 60h 72h 84h 10^-2 10^-3 10^-4 10^-1 10^-2 10^-3 10^-1 10^-2 10^-3 10^-1 10^-1 10^-1 10^-1 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-1 10^-2 10^-3 10^-4 10^-1 10^-2 10^-3 10^-1 10^-2 10^-3 10^-1 10^-1 10^-1 10^-1 105 7 -- ---- --- 57 5 -TNTC TNTC 19 17 1 2 222 350 3 3 1 0 107 89 16 12 3 5 0 0 Rep 2 09/18/12 Plate 1 Plate 2 TNTC TNTC 119 132 13 32 3 5 236 297 22 18 2 1 4 0 29 17 2 0 -1 0 --1 0 0 0 --- 1800 3.26 2860 3.46 980 140 40 <5 2.99 2.15 1.60 <0.70 Survivors 19033 Log CFU/ml 4.28 2665 3.43 230 2.36 5 0.70 5 <5 0.70 <0.70 89 Appendix VI. Juice Variables Raw Data, Chapter 3. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/ml or 0.70 Log CFU/ml. Table VI.1 E. coli O157:H7 in 'Marion' Juice with added ethanol, Raw Data 08/22/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 191 80 7 TNTC TNTC 169 43 12 397500 5.60 TNTC TNTC 184 41 1 TNTC TNTC 131 42 6 286250 5.46 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors TNTC TNTC 135 82 58 40 1 0 --12h 29925 4.48 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Dilution on Plate 10^-1 Plate 1 38 1 0 0 0 36h 10^-2 10^-3 10^-4 10^-5 Dilution on Plate 10^-1 Plate 1 10^-2 ----- 10^-3 10^-4 10^-5 TNTC TNTC Error Error Error Error Error Error --24h Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 27 0 0 0 0 325 2.51 1 0 5 0.70 ----Survivors 0 ----- Log CFU/ml Plate 2 Plate 2 0 6h <5 Log CFU/ml <0.70 ----- 90 Table VI.2 E. coli O157:H7 in 'Black Diamond' Juice with added ethanol, Raw Data 08/22/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 152 37 5 TNTC TNTC 141 21 7 221000 5.34 TNTC TNTC 77 10 2 TNTC TNTC 95 9 1 86000 4.93 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 107 194 54 40 7 5 --- 31025 4.49 TNTC TNTC 45 28 5 3 1 0 --- 3650 3.56 Survivors Log CFU/ml 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 24h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 114 11 2 0 0 80 11 0 0 0 970 2.99 2 0 Plate 1 Plate 2 Survivors Log CFU/ml 0 <5 <0.70 ---- 10 1.00 ---- 36h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 0 ---- ---- Table VI.3 Salmonella Typhimurium in 'Marion' Juice with added ethanol, Raw Data 08/14/2012 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 169 3 0 0 0 192 10 0 0 0 1805 3.26 97 1 0 0 0 90 0 0 0 0 935 2.97 91 4h Dilution on Plate 10^-1 6h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 2 0 0 0 0 3 0 0 0 0 25 1.40 0 0 0 0 0 0 0 0 0 0 <5 <0.70 10^-2 10^-3 10^-4 10^-5 Table VI.4 Salmonella Typhimurium in 'Black Diamond' Juice with added ethanol , Raw Data 08/14/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 15 1 0 0 0 12 0 0 0 0 135 2.13 1 0 0 0 0 5 0 0 0 0 30 1.48 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 1 0 0 0 0 0 0 0 0 0 5 0.70 0 0 0 0 0 0 0 0 0 0 <5 0.70 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h Table VI.5 L. monocytogenes in 'Marion' Juice with added ethanol, Raw Data 09/05/12 0.5h 1h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC 41 1 1 0 TNTC 58 7 0 0 4950 3.69 20 0 0 0 0 25 0 0 0 0 22.5 1.35 Plate 1 Plate 2 Survivors Log CFU/ml 2h Dilution on Plate 92 10^-1 10^-2 10^-3 10^-4 10^-5 0 0 0 0 0 0 0 0 0 0 <5 <0.70 Table VI.6 L. monocytogenes in 'Black Diamond' Juice with added ethanol , Raw Data 09/05/12 0.5h 1h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 22 0 0 0 0 29 0 0 0 0 25.5 1.41 0 0 0 0 0 0 0 0 0 0 <5 <0.70 Table VI.7 S. aureus in 'Marion' Juice with added ethanol , Raw Data 09/18/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 95 16 0 TNTC TNTC 73 15 1 84000 4.92 TNTC 193 58 9 0 TNTC 203 39 11 0 34150 4.53 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 101 72 12 3 0 0 --- 8650 3.94 TNTC TNTC 50 61 5 2 0 0 --- 5550 3.74 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 24h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 16 2 0 0 6 0 0 0 110 2.04 0 0 <5 <0.70 ---- ---- 93 10^-5 -- -- -- -- Table VI.8 S. aureus in 'Black Diamond' Juice with added ethanol , Raw Data 09/18/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 143 35 2 TNTC TNTC 108 42 0 255250 5.41 TNTC 243 92 20 0 TNTC TNTC 102 20 0 72767 4.86 Plate 2 Survivors Log CFU/ml TNTC TNTC 101 65 13 10 4 0 --- 8300 3.92 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 6h Plate 2 Survivors Log CFU/ml TNTC TNTC 160 171 10 3 0 1 --- 16550 4.22 Plate 1 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 24h Plate 1 Plate 2 Survivors Log CFU/ml 100 13 0 0 79 8 0 0 895 2.95 -- 10^-2 10^-3 10^-4 10^-5 ----- -Plate 1 Plate 2 Survivors Log CFU/ml 0 0 <5 <0.70 ----- 6 ---- 36h Dilution on Plate 10^-1 Plate 1 ---- Plate 2 Survivors Log CFU/ml 4 50 1.70 94 Appendix VII. Wine Raw Data, Chapter 3. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/ml or 0.70 Log CFU/ml. Table VII.1 E. coli O157:H7 in 'Marion' Wine, Raw Data Rep 1 12/09/11 10m Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC 194 38 3 1 0 TNTC 190 43 2 0 0 29850 4.47 91 3 0 0 0 0 112 0 0 0 0 0 1015 3.01 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 222 ----- 22200 4.35 Rep 1 12/09/11 40m Dilution on Plate 10^-1 Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 0 0 0 0 0 0 <5 <0.70 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 87 TNTC TNTC TNTC 68 775000 5.89 Plate 1 Plate 2 Survivors Log CFU/ml 36 375 2.57 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 2 07/30/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10m Rep 2 07/30/12 10^-3 10^-4 20m 40m Dilution on Plate 10^-1 10^-2 20m 39 ---- ---- 60m Plate 1 0 ---- ---- Plate 2 Survivors Log CFU/ml 0 <5 <0.70 95 Table VII.2 E. coli O157:H7 in 'Black Diamond' Wine, Raw Data Rep 1 10m 12/09/11 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 1 12/09/11 Dilution on Plate 10^-1 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 197 67 10 1 TNTC TNTC 182 74 12 3 447250 5.65 240 113 17 0 0 0 232 104 14 0 0 0 6605 3.82 40m Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 0 0 0 0 0 0 <5 <0.70 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 2 07/30/12 Dilution on Plate 10^-1 10m Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 30 5 1 0 42 8 1 0 360 2.56 0 0 0 0 0 0 0 0 <5 <0.70 10^-3 10^-4 10^-2 10^-3 10^-4 20m Plate 1 10^-2 Rep 2 07/30/12 Dilution on Plate 10^-1 20m 40m Plate 1 ----- Plate 2 ----- -- -- 96 Table VII.3 Salmonella Typhimurium in 'Marion' Wine, Raw Data Rep 1 10m 12/07/11 Dilution on Plate 10^-1 Plate 1 Plate 2 Survivors 248 23 1 0 0 0 262 35 0 0 0 0 2760 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 1 12/07/11 Dilution on Plate 10^-1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 0 0 0 0 0 0 <5 <0.70 10^-4 10^-5 10^-6 10^-3 Rep 2 07/22/12 Dilution on Plate 10^-1 10^-2 10^-3 Plate 2 3 0 0 0 0 0 1 0 0 0 0 0 3.44 Plate 1 10^-3 10^-2 Plate 1 10^-2 10^-3 Log CFU/ml 20 1.30 Plate 2 Survivors Log CFU/ml 52 480 2.68 10m 20m Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 51 TNTC TNTC 37 44000 4.64 Plate 1 44 --- --- 40m Plate 1 Plate 2 Survivors Log CFU/ml 0 0 <5 <0.70 --- --- Table VII. 4 Salmonella Typhimurium in 'Black Diamond' Wine, Raw Data Rep 1 10m 12/07/11 Dilution on Plate 10^-1 Survivors 40m 10^-2 Rep 2 07/22/12 Dilution on Plate 10^-1 Log CFU/ml 20m 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 204 TNTC TNTC 189 365750 5.56 TNTC 263 51 TNTC 205 60 43833 4.64 97 10^-4 65 2 0 10^-5 10^-6 Rep 1 12/07/11 Dilution on Plate 10^-1 Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 0 0 0 0 0 0 <5 <0.70 10^-3 10^-4 10^-5 10^-6 10^-2 10^-3 Rep 2 07/22/12 Dilution on Plate 10^-1 10^-2 10^-3 7 1 0 7 2 0 40m 10^-2 Rep 2 07/22/12 Dilution on Plate 10^-1 42 10 0 10m 20m Plate 1 Plate 2 Survivors Log CFU/ml TNTC 173 23 TNTC 151 23 16200 4.21 Plate 1 Plate 2 1 --- 0 10^-2 10^-3 10^-4 10^-5 10^-6 0.70 40m Plate 1 Plate 2 Survivors 0 <5 0 --- Log CFU/ml <0.70 --- 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 159 10 4 TNTC TNTC TNTC 176 17 1 1675000 6.22 TNTC TNTC 294 51 3 0 TNTC TNTC 286 33 2 0 420000 5.62 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 54 47 505 2.70 0 0 <5 <0.70 Rep 1 Dilution on Plate 10^-1 5 Log CFU/ml --- Table VII.5 L. monocytogenes in 'Marion' Wine, Raw Data Rep 1 10m 02/08/12 Dilution on Plate 10^-1 Survivors 40m 60m 98 10^-2 4 0 0 0 0 10^-3 10^-4 10^-5 10^-6 Rep 2 08/01/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 3 0 0 0 0 10^-2 10^-3 10^-4 10^-5 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 172 20 TNTC TNTC TNTC 201 30 2243333 6.35 TNTC TNTC TNTC 93 10 TNTC TNTC TNTC 127 8 1100000 6.04 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 246 320 ------- 28300 4.45 0 10 1.00 40m Rep 2 60m Plate 2 Survivors Log CFU/ml 0 0 <5 <0.70 10^-2 ----- 10^-5 ----- 80m Plate 1 10^-4 2 ----- Dilution on Plate 10^-1 10^-3 0 0 0 0 0 10m Rep 2 Dilution on Plate 10^-1 0 0 0 0 0 ----- Table VII.6 L. monocytogenes in 'Black Diamond' Wine, Raw Data Rep 1 10m 02/16/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 120 15 1 TNTC TNTC TNTC 114 11 0 1170000 6.07 TNTC TNTC 57 11 0 0 TNTC TNTC 43 16 1 0 50000 4.70 99 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 2 08/01/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 40m Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 0 0 0 0 0 0 <5 <0.70 10m 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 104 73 7 3 0 181 102 19 4 0 5088 3.71 0 0 0 0 0 0 0 0 0 0 <5 <0.70 Table VII.7 S. aureus in 'Marion' Wine, Raw Data Rep 1 10m 02/14/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC 150 36 7 0 0 TNTC 221 35 15 0 0 27025 4.43 TNTC 94 32 17 0 0 TNTC 176 37 2 0 0 24000 4.38 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 162 26 7 0 0 0 185 25 2 0 1 0 2143 3.33 4 3 0 0 0 0 3 1 0 0 0 0 35 1.54 Rep 1 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-6 40m Rep 1 Dilution on Plate 20m 60m 80m Plate 1 Plate 2 Survivors Log CFU/ml 100 10^-1 0 0 0 0 0 0 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 2 07/22/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 0 0 0 0 0 0 Plate 2 Survivors Log CFU/ml TNTC TNTC 240 65 3 TNTC TNTC 180 40 3 367500 5.57 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 6 4 0 13 3 1 95 1.98 0 0 <5 <0.70 --- Log CFU/ml TNTC TNTC TNTC TNTC 178 231 27 31 --- 247250 5.39 ----- 80m Plate 1 Plate 2 Survivors Log CFU/ml 0 0 <5 <0.70 10^-2 ----- 10^-5 Survivors ----- Dilution on Plate 10^-1 10^-4 Plate 2 60m --- Rep 2 10^-3 Plate 1 40m 10^-3 10^-5 20m Plate 1 10^-2 10^-4 0.70 10m Rep 2 Dilution on Plate 10^-1 <5 ----- Table VII.8 S. aureus in 'Black Diamond' Wine, Raw Data Rep 1 10m 02/23/12 Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 20m Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 159 24 2 TNTC TNTC 99 22 1 129000 5.11 TNTC TNTC 122 23 0 TNTC TNTC 101 7 0 11500 5.05 101 10^-6 0 0 Plate 1 5876.66 7 Survivors 375 51 6 2 0 0 311 33 14 0 0 0 Rep 1 10^-2 10^-3 10^-4 10^-5 10^-6 Rep 1 Plate 1 Plate 2 0 0 0 0 0 0 0 0 0 0 0 0 10^-2 10^-3 10^-4 10^-5 10^-6 10^-3 10^-4 10^-5 10^-4 4200 3.77 1 0 0 0 0 0 2 0 0 0 0 0 15 1.18 Survivors Log CFU/ml <5 <0.70 20m Log CFU/ml TNTC TNTC 161 21 3 TNTC TNTC 168 16 4 164500 5.22 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 181 168 23 31 1 3 --- 11497 4.06 40m Plate 1 Plate 2 6 0 0 --- 60m Survivors 2 1 0 40 Log CFU/ml ---- Plate 1 Plate 2 Survivors Log CFU/ml 0 0 <5 <0.70 Plate 2 0 ----- --- ---- Plate 1 1.60 80m Dilution on Plate 10^-1 10^-3 Log CFU/ml Survivors Rep 2 10^-2 Survivors 60m Plate 2 10^-3 10^-5 Plate 2 Plate 1 10^-2 10^-4 Plate 1 10m Rep 2 Dilution on Plate 10^-1 Log CFU/ml 80m Dilution on Plate 10^-1 10^-2 0 40m Dilution on Plate 10^-1 Rep 2 07/22/12 Dilution on Plate 10^-1 0 Survivors 0 ----- <5 Log CFU/ml <0.70 102 10^-5 -- -- Appendix VIII. Wine Variable Raw Data, Chapter 3. Bold indicates value used in calculation. Detection limit calculated as: <1 colony/plate at the lowest dilution with 0.1 ml on each of 2 plates 1/0.2 = 5 CFU/ml or 0.70 Log CFU/ml. Table VIII.1 E. coli O157:H7 in pH adjusted 'Marion' Wine, Raw Data 07/30/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC TNTC 184 TNTC 88 58 5 19 54800 5.74 TNTC TNTC TNTC 56 6 TNTC TNTC TNTC 46 10 510000 5.70 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 153 75 10 TNTC TNTC 221 79 10 478500 5.68 TNTC TNTC 100 49 3 TNTC TNTC 188 51 3 322000 5.51 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC 45 18 3 0 TNTC 88 3 2 0 6650 3.82 19 0 0 34 0 0 265 2.42 Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 <5 <0.70 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 24h --36h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 ---- ---- --- 103 Table VIII.2 E. coli O157:H7 in pH adjusted 'Black Diamond' Wine, Raw Data 07/30/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 115500 0 6.06 TNTC TNTC 665000 5.82 TNTC TNTC 134 15 TNTC TNTC 97 16 TNTC TNTC 74 2 TNTC TNTC 59 11 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC 78 10 TNTC TNTC 223 72 6 574333 5.76 TNTC TNTC 122 38 3 TNTC TNTC 259 40 2 300667 5.48 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 24h Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 46 10 0 TNTC 131 41 13 0 33367 4.52 Plate 1 Plate 2 Survivors Log CFU/ml 10 0 0 54 0 0 320 2.51 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 59 35 10 5 ----- 4700 3.67 36h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 --- 48h Plate 1 Survivors Log CFU/ml 0 <5 <0.70 0 ----- --- Plate 2 ----- Table VIII.3 Salmonella Typhimurium in pH adjusted 'Marion' Wine, Raw Data 07/22/12 6h Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 Survivors Log CFU/ml 0 0 0 0 0 0 <5 <0.70 104 Table VIII.4 Salmonella Typhimurium in pH adjusted 'Black Diamond' Wine, Raw Data 07/22/12 6h 12h Dilution on Plate 10^-1 10^-2 10^-3 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 8 0 0 8 0 0 80 1.90 9 3 60 1.78 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 1 0 5 0.70 0 0 <5 <0.70 --- --- 24h Dilution on Plate 10^-1 10^-2 10^-3 --- 36h --- --- --- Table VIII.5 L. monocytogenes in pH adjusted 'Marion' Wine, Raw Data 08/01/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 127500 0 6.11 TNTC TNTC 463000 5.67 TNTC TNTC 156 8 TNTC TNTC 99 7 TNTC TNTC 55 4 TNTC 189 65 6 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 6h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 223 16 1 TNTC TNTC 112 20 0 167500 5.22 TNTC TNTC 78 16 0 TNTC TNTC 67 7 0 72500 4.86 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 179000 5.25 TNTC TNTC 31766.6 7 4.50 TNTC 170 26 TNTC 188 8 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 24h TNTC 123 56 27 --- 105 10^-5 0 0 -- -- Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 105 81 12 12 ----- 9300 3.97 39 16 32 24 355 2.55 36h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 48h ---- ---- Table VIII.6 L. monocytogenes in pH adjusted 'Black Diamond' Wine, 08/01/12 1h 2h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 TNTC TNTC 147500 0 6.17 TNTC TNTC TNTC TNTC 163 2 TNTC TNTC 132 8 TNTC 325 63 3 TNTC TNTC 25 2 Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 174 25 1 TNTC TNTC 201 8 1 208333 5.32 TNTC TNTC 140 27 0 TNTC TNTC 162 1 0 190667 5.28 4h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 10^-2 10^-3 10^-4 10^-5 10^-2 10^-3 5.64 24h Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 227 26 2 TNTC TNTC 111 15 0 199333 5.30 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC TNTC TNTC 92 21 ----- 56500 4.75 36h Dilution on Plate 10^-1 440000 Log CFU/ml 6h 12h Dilution on Plate 10^-1 Survivors 48h Plate 1 Plate 2 Survivors Log CFU/ml TNTC 150 38 TNTC 203 7 24433 4.39 Plate 1 Plate 2 Survivors Log CFU/ml TNTC TNTC 142 181 --- 16150 4.21 106 10^-4 10^-5 --- --- --- --- Table VIII.7 S. aureus in pH adjusted 'Marion' Wine, Raw Data 07/22/12 6h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 12h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 253 18 0 0 0 180 41 0 0 0 2950 3.47 61 2 0 0 0 21 1 0 0 0 410 2.61 24h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 Plate 1 Plate 2 1 0 0 0 --- 36h Survivors 5 Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 0.70 0 0 <5 <0.70 Survivors Log CFU/ml ---- --- ---- 10^-5 Table VIII.8 S. aureus in pH adjusted 'Black Diamond' Wine, Raw Data 07/22/12 6h 12h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 Plate 1 Plate 2 116 5 2 0 0 136 24 1 0 0 Survivors 1260 Log CFU/ml Plate 1 Plate 2 3.10 15 0 0 0 0 19 0 0 0 0 24h Dilution on Plate 10^-1 10^-2 10^-3 10^-4 10^-5 2.23 36h Plate 1 Plate 2 Survivors Log CFU/ml Plate 1 Plate 2 Survivors Log CFU/ml 2 0 0 0 0 0 0 0 0 0 10 1.00 2 0 10 1.00 Plate 1 Plate 2 ----48h Dilution on Plate 170 Survivors Log CFU/ml ----- 107 10^-1 0 10^-2 ----- 10^-3 10^-4 10^-5 0 <5 <0.70 ----- Appendix IX. Inocula Raw Data, Chapter 3. Bold indicates value used for calculation. Table IX.1 Inocula for Juice Survival Studies (Log CFU/ml represents 100 µl of inoculum used) E. coli O157:H7 12/14/11 E. coli O157:H7 08/22/12 Dilution on Plate 10^-6 Plate 1 Plate 2 CFU/ml 85 82 83500000 10 11 835000 10^-8 2 1 Salmonella Typhimurium 12/14/11 10^-7 Dilution on Pate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-5 10^-6 10^-7 Dilution on Plate 10^-6 10^-7 10^-8 Plate 1 Plate 2 CFU/ml 85 75 80000000 8 13 800000 1 0 L. monocytogenes 03/03/12 Plate 1 Plate 2 CFU/ml 208 199 245666667 33 24 2456667 2 3 S. aureus 03/23/12 Plate 1 Plate 2 CFU/ml 267 232 37733333 36 54 377333 7 4 S. aureus 09/18/12 Plate 1 Plate 2 CFU/ml 116 6 1 136 15 2 126000000 1260000 Log CFU/ml Plate 1 Plate 2 CFU/ml Log CFU/ml 124 117 240250000 5.92 36 36 2402500 4 2 Salmonella Typhimurium 08/14/12 Log CFU/ml 5.90 Log CFU/ml 6.39 Log CFU/ml 5.58 Log CFU/ml 6.10 Plate 1 62 14 3 Plate 1 272 33 8 Plate 2 CFU/ml 6.38 Log CFU/ml 57 59500000 7 595000 5.77 2 L. monocytogenes 09/05/12 Plate 2 CFU/ml 295 345000000 36 3450000 6 S. aureus 04/11/12 Log CFU/ml 6.54 Plate 1 Plate 2 CFU/ml Log CFU/ml 268 40 6 263 58 4 49000000 490000 5.69 108 Table IX.2 Inocula for Wine Survival Studies (Log CFU/ml Represents 100 µl of inoculum used) E. coli O157:H7 12/09/11 E. coli O157:H7 07/30/12 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Dilution on Plate 10^-6 10^-7 10^-8 Plate 1 Plate 2 CFU/ml Log CFU/ml 109 98 103500000 18 12 1035000 6.01 1 0 Salmonella Typhimurium 12/07/11 Plate 1 107 17 3 Plate 1 165 22 0 Plate 1 TNTC 139 1 Plate 1 Plate 2 CFU/ml Log CFU/ml Plate 1 Plate 2 CFU/ml Log CFU/ml 102 136 166000000 26 20 1660000 6.22 2 3 Salmonella Typhimurium 07/22/12 Plate 1 Plate 2 CFU/ml Log CFU/ml 104 105500000 TNTC TNTC 245000000 19 1055000 6.02 22 27 2450000 6.39 3 0 2 L. monocytogenes 02/08/12 L. monocytogenes 02/16/12 Plate 2 Log CFU/ml Plate 1 Plate 2 CFU/ml 158 161500000 21 1615000 6.21 0 L. monocytogenes 08/01/12 155 22 1 159 15 1 157000000 1570000 Plate 2 CFU/ml CFU/ml TNTC 1465000000 154 14650000 1 S. aureus 02/14/12 Plate 2 CFU/ml 27 18 22500000 7 0 225000 0 0 S. aureus 07/22/12 Plate 1 Plate 2 CFU/ml 96 4 1 59 11 0 77500000 775000 Log CFU/ml 6.20 Log CFU/ml 7.17 S. aureus 02/23/12 Log CFU/ml Plate 1 Plate 2 CFU/ml 5.35 28 3 1 12 3 1 20000000 200000 Log CFU/ml 5.89 Log CFU/ml 5.30